CN111889869A - Welding method for high-purity rare earth and alloy target - Google Patents
Welding method for high-purity rare earth and alloy target Download PDFInfo
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Abstract
The invention discloses a welding method of high-purity rare earth and alloy target materials, belonging to the technical field of target material welding, comprising the following steps: carrying out gear turning on the welding surfaces of the rare earth target blank and the back plate, and carrying out back gold treatment on the gear turning surface; plating a protective layer on the non-welding surface of the rare earth target blank; an intermediate layer is arranged on the welding interface of the two; preparing a sheath for welding, and coating a protective layer on the inner surface of the sheath; assembling the rare earth target blank, the intermediate layer and the back plate into a sheath, and performing electron beam sealing processing on the sheath to obtain a sealing welding target material; and carrying out hot isostatic pressure diffusion welding on the seal welding target material to obtain the high-purity rare earth target material. The target material prepared by the invention overcomes the problems of high activity, easy oxidation and reaction pollution with sheath materials of rare earth materials, the target material welding rate is more than or equal to 99 percent, the welding strength is more than or equal to 60MPa, and the sheath and the target material can be automatically separated, thereby saving the cost and improving the production efficiency.
Description
Technical Field
The invention belongs to the technical field of target welding, and particularly relates to a welding method of a high-purity rare earth and alloy target.
Background
With the continuous development of the integrated circuit industry technology, the size of the CMOS transistor is smaller and smaller, the integration level is higher and higher, and SiO is often adopted when the process node is about 65nm2A material; when the process node is 45-14nm, the hafnium-based composite material is used; at the process node below 10nm, the hafnium-based composite material cannot meet the process requirements, and a higher-K gate dielectric material or a rare earth high-K gate dielectric material is required to be adopted, for example: the amorphous oxide of lanthanum, yttrium, gadolinium and other elements has the characteristics of high dielectric constant, large band gap, good thermal stability and the like, and therefore, the amorphous oxide becomes an excellent substitute material for the gate dielectric material of the next-generation integrated circuit. Rare earth alloy targets, such as high-purity aluminum-scandium-rare earth alloy targets, are mainly used for sputtering high-purity AlScN films. Compared with the existing AlN piezoelectric film, the AlN piezoelectric film has stronger and better piezoelectric performance, and the application fields of the AlN piezoelectric film are mainly divided into the manufacture of high-frequency mobile communication (5G) radio frequency filter chips and various advanced MEMS sensors.
The preparation of films such as gate dielectric materials and the like generally adopts a PVD magnetron sputtering technology, and adopts raw materials as corresponding sputtering targets. The development of high-purity rare earth metal target materials has important significance for solving the urgent need of advanced electronic materials. For the preparation process of the target material, the target material and the back plate are generally welded and formed, and then are subjected to machining and post-treatment processes to obtain a finished target material product.
Rare earth materials are rare resources, high-purity rare earth materials are expensive, targets can be welded with sheath materials after target diffusion welding, and are very difficult to remove, meanwhile, after target diffusion welding, the targets can deform to different degrees due to different linear expansion coefficients of the targets, a back plate and the sheath materials, when the sheath is removed by machining, part of rare earth materials can be removed by machining, so that resource waste is caused, meanwhile, the thickness uniformity of the targets is poor, and the performance of the ferromagnetic rare earth materials is reduced.
The high-purity rare earth material is easy to react with air and water due to high activity, and is easy to react with materials such as solder indium, metal aluminum, copper and the like at high temperature, so that higher requirements are put on a welding process in a processing process. At present, there are few reports about scientific research and industrial application of rare earth target welding technology at home and abroad.
Disclosure of Invention
In order to solve the problems, the invention provides a welding method of a high-purity rare earth and alloy target, which comprises the following steps:
1) processing a rare earth target blank and a back plate: carrying out gear turning on the welding surfaces of the rare earth target blank and the back plate, carrying out back gold treatment on the gear turning surface, and then carrying out vacuum packaging;
2) surface treatment of the rare earth target blank: plating a protective layer on the non-welding surface of the rare earth target blank;
3) designing an intermediate layer: arranging an intermediate layer on a welding interface of the rare earth target blank and the back plate;
4) and (3) sheath processing: preparing a sheath for welding by a common vehicle, and cleaning the sheath before welding;
5) special treatment of sheathing: uniformly coating a protective layer on the inner surface of the sheath, and drying;
6) and (3) electron beam seal welding processing: assembling the rare earth target blank, the intermediate layer and the back plate into a sheath, and performing electron beam sealing welding processing on the sheath interface under a vacuum condition to obtain a sealing welding target material;
7) hot isostatic pressing diffusion welding processing: and (3) carrying out hot isostatic pressure diffusion welding processing on the seal welding target material, biting the turning tooth structures of the rare earth target blank and the back plate into the intermediate layer material, carrying out diffusion welding, and removing the sheath to obtain the integrated high-purity rare earth target material.
The rare earth material of the high-purity rare earth target comprises: any one of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium metal, and alloys thereof; the alloy comprises rare earth Al alloy, Fe alloy, Co alloy or Zr alloy; the method specifically comprises the following steps: alloys such as Nb-Fe, Sm-Fe, Tb-Fe, Dy-Fe, Al-Sc, Al-Nd, Al-Er, Co-Zr-RE and the like; the back plate material comprises aluminum alloy, copper or copper alloy; the welding rate of the high-purity rare earth target material is more than or equal to 99 percent, and the welding strength is more than or equal to 60 MPa.
The protective layer material in the step 5) is BN or ZrO2。
The protective layer material in the step 2) is TaN or TiN.
The back gold method in the step 1) adopts a magnetron sputtering coating method, and the sputtered film is a high-purity Ni or NiV film.
The vehicle tooth structure in the step 1) is formed by distributing V-shaped depressions and trapezoidal convex parts at intervals, the bottom angle alpha of each V-shaped depression is 55 degrees, and two sides of each V-shaped depression are symmetrical about a bisector of the bottom angle; the depth h of the V-shaped concave part and the trapezoidal convex part is 0.2 cm; the length L of every two adjacent V-shaped depressions and trapezoidal convex parts is 0.35 cm.
The material of the intermediate layer in the step 3) is pure aluminum or titanium, and the thickness is 1.8-8 mm.
And 4) adopting 6061Al or stainless steel as a sheath material in the step 4), and carrying out acid washing treatment on the sheath by using dilute hydrochloric acid to remove a surface oxide layer.
And 6) carrying out electron beam seal welding processing in a vacuum environment.
The welding temperature in the step 7) is 250-.
The invention has the beneficial effects that:
1. the welding method for preparing the rare earth target has high welding strength, is suitable for the requirement of high sputtering power, and is suitable for the fields of semiconductor and integrated circuit manufacturing and the like.
2. The rare earth material with high activity is protected by adopting a method of sputtering a protective layer material, so that the rare earth material is prevented from reacting or diffusing with a sheath material or a protective material, the pollution and even scrapping of the rare earth material are avoided, the utilization rate of the rare earth material is improved, the feeding is reduced, and the cost is saved.
3. The invention coats the inner surface of the sheath with BN or ZrO2The materials are protected and treated, so that the covering is avoidedReaction or diffusion with rare earths, coatings or backsheets; when the sheath is removed, the sheath and the target can be automatically separated, so that the situation that part of rare earth materials are removed due to welding deformation during sheath processing is avoided, the thickness uniformity of the rare earth target is ensured, for the rare earth and the alloy target with ferromagnetism, the influence of the thickness uniformity of the target on the permeability uniformity of the material is large, the higher the thickness uniformity of the target is, and the better the uniformity of the prepared film is; the common methods for preparing the coating are plasma spraying, physical chemical vapor deposition, self-propagating high-temperature combustion synthesis and the like, the technical equipment is complex, the cost is high, the method adopts a simple physical coating mode to prepare the protective material, the operation is simple, the cost is low, the efficiency is high, the rare earth target can be effectively protected, and the processing efficiency and the target performance are effectively improved.
4. The welding method of the invention overcomes the problems of high activity of rare earth materials and welding oxidation of the conventional brazing welding method, and simultaneously avoids the reaction pollution of the rare earth materials and the welding flux.
5. In order to overcome the problem of low direct welding strength of the target and the back plate, the invention introduces the design of an intermediate layer welding interface to carry out the design of a welding surface structure and a back metal, and optimally selects an intermediate layer material to realize the high-reliability connection of the target and the back plate.
6. According to the invention, through structural design of a welding interface, metallization of the target material and protection treatment of the sheath, the welding rate and the welding strength of the target material are improved, the welding rate is more than or equal to 99%, the welding strength is more than or equal to 60MPa, the rare earth target material is effectively protected, no reaction and diffusion pollution are generated with the sheath, the sheath and the target material can be automatically separated, the cost is saved, and the production efficiency is improved.
Drawings
FIG. 1 is a flow chart of a target diffusion welding process;
FIG. 2 is a front view of a target blank;
FIG. 3 is a top view of a target blank;
FIG. 4 is an enlarged view of a portion A of FIG. 2;
FIG. 5 is a schematic diagram of a jacket structure;
FIG. 6 is a view of a target weld pattern including an interlayer material;
FIG. 7 is an enlarged view of the target welding structure shown in part A of FIG. 6;
FIG. 8 is a view of a target weld without interlayer material;
FIG. 9 is an enlarged view of the target welding structure shown in part A of FIG. 8;
wherein:
1-target blank, 2-backboard, 3-intermediate layer, 4-sheath.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples: processing according to the flow chart shown in figure 1:
1) processing a rare earth target blank and a back plate: performing annular gear turning on the welding surface of the rare earth target blank and the back plate by taking the center as an original point, wherein the gear turning structure and the position are shown in figures 2, 3 and 4, the gear turning structure is formed by V-shaped depressions and trapezoidal convex parts which are distributed at intervals, the bottom angle of each V-shaped depression is alpha, the angle is 55 degrees, and the two sides of each angle are symmetrical about the bisector of the bottom angle; the depth h of the V-shaped recess is 0.2 cm; the length L of every two adjacent V-shaped depressions and trapezoidal convex parts is 0.35 cm.
And two exhaust grooves are processed in the direction vertical to the annular lathed teeth. The included angle of the two exhaust grooves is 90 degrees, so that the gas in the ladle sleeve in the subsequent step 6) of electron beam seal welding processing can be effectively discharged, and the welding effect and the firmness are improved.
Then carrying out back gold treatment on the gear surface; then the rare earth materials are subjected to 2-layer vacuum packaging to prevent oxidation or pollution.
2) Surface treatment of the rare earth target blank: and plating a protective layer on the non-welding surface of the rare earth target blank.
3) Designing an intermediate layer: in order to achieve high-strength welding of the target material and the back plate, an intermediate layer is arranged on a welding interface of the rare earth target blank and the back plate; and realizing the reliable connection of the target blank and the back plate.
4) And (3) sheath processing: preparing a sheath for welding by a common vehicle, wherein the sheath structure is shown in figure 5 and comprises an upper sheath and a lower sheath which are detachable, the upper sheath and the lower sheath are of cylindrical structures, the bottom surface of one end of the upper sheath is closed, the other end of the upper sheath is opened, and the shape of the bottom surface is matched with that of a finished target material; the upper and lower sheath are clamped, and the whole body is in a closed state; and cleaning the sheath before welding.
5) Special treatment of sheathing: uniformly coating a protective layer on the inner surface of the sheath, and drying; and carrying out surface protection treatment on the inner surface of the sheath.
6) Electron beam seal welding (EB) processing: during use, the rare earth target blank, the intermediate layer and the back plate are sequentially assembled in the lower sheath, the position is adjusted, the upper sheath is covered, the upper sheath and the lower sheath are clamped, and the whole body is in a closed state; and carrying out electron beam sealing and welding processing on the clamping circumference to obtain the sealing and welding target material.
7) Hot isostatic pressure diffusion welding (HIP) processing: and (3) carrying out hot isostatic pressing diffusion welding processing on the seal welding target material, biting the lathing tooth structures of the target blank and the back plate into the intermediate layer material (see figures 6 and 7), and carrying out diffusion welding to obtain the integrated high-purity rare earth target material.
Example one
Machining according to the machining process flow chart shown in FIG. 1, namely, carrying out tooth turning on the welding surface of the rare earth Y target blank, carrying out Ni back-gold treatment, protecting the back-gold surface, and carrying out sputtering plating of a protective material TaN on other surfaces of the rare earth target blank; the back plate adopts copper alloy C18000, and the welding surface of the back plate is processed by gear turning (the gear turning structure is shown in figure 2) and Ni back gold processing is carried out; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal-welded target material, wherein the HIP pressure is 90MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 3h, after welding processing, the sheath and the rare earth Y target material have no reaction and diffusion pollution, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The welding structure of the interlayer material with the target blank and the backing plate is shown in fig. 6 and 7, and the welding rate and the welding strength data are shown in table 1.
Example two
Turning teeth on the welding surface of the rare earth Y target blank, carrying out Ni back-gold treatment, protecting the back-gold surface, and carrying out sputtering plating of a protective material TaN on other surfaces of the rare earth Y target blank; the back plate adopts copper alloy C18000, and the welding surface of the back plate is subjected to gear turning and Ni back gold treatment; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal-welded target material, wherein the HIP pressure is 100MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 3h, after welding processing, the sheath and the rare earth Y target material have no reaction and diffusion pollution, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
EXAMPLE III
Turning teeth on the welding surface of the rare earth Y target blank, carrying out Ni back-gold treatment, protecting the back-gold surface, and carrying out sputtering plating of a protective material TaN on other surfaces of the rare earth Y target blank; the back plate adopts copper alloy C18000, and the welding surface of the back plate is subjected to gear turning and Ni back gold treatment; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and performing HIP welding processing on the seal-welded target material, wherein the HIP pressure is 110MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 3h, the sheath and the rare earth Y target material have no reaction and diffusion pollution after welding processing, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Example four
Turning teeth on the welding surface of the rare earth Y target blank, carrying out Ni back-gold treatment, protecting the back-gold surface, and carrying out sputtering plating of a protective material TaN on other surfaces of the rare earth Y target blank; the back plate adopts copper alloy C18000, and the welding surface of the back plate is subjected to gear turning and Ni back gold treatment; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal-welded target material, wherein the HIP pressure is 100MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 4h, after welding processing, the sheath and the rare earth Y target material have no reaction and diffusion pollution, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
EXAMPLE five
Turning teeth on the welding surface of the rare earth Y target blank, carrying out Ni back-gold treatment, protecting the back-gold surface, and carrying out sputtering plating of a protective material TaN on other surfaces of the rare earth Y target blank; the back plate adopts copper alloy C18000, and the welding surface of the back plate is subjected to gear turning and Ni back gold treatment; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal-welded target material, wherein the HIP pressure is 100MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 5h, the sheath and the rare earth Y target material have no reaction and diffusion pollution after welding processing, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
EXAMPLE six
Turning teeth on the welding surface of the rare earth Y target blank, carrying out Ni back-gold treatment, protecting the back-gold surface, and carrying out sputtering plating of a protective material TaN on other surfaces of the rare earth Y target blank; the back plate adopts copper alloy C18000, and the welding surface of the back plate is subjected to gear turning and Ni back gold treatment; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 400 ℃, the heat preservation and pressure maintaining time is 4h, after welding processing, the sheath and the rare earth Y target material have no reaction and diffusion pollution, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
EXAMPLE seven
Turning teeth on the welding surface of the rare earth Y target blank, carrying out Ni back-gold treatment, protecting the back-gold surface, and carrying out sputtering plating of a protective material TaN on other surfaces of the rare earth Y target blank; the back plate adopts copper alloy C18000, and the welding surface of the back plate is subjected to gear turning and Ni back gold treatment; the intermediate layer is made of 1060Al material with the thickness of 2 mm; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 500 ℃, the heat preservation and pressure maintaining time is 4h, after welding processing, the sheath and the rare earth Y target material have no reaction and diffusion pollution, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Example eight
Protecting the welding surface of the rare earth Gd target blank, and sputtering and plating a protective material TaN on other surfaces of the rare earth target blank; the back plate adopts copper alloy CuCr1, and the welding surface of the back plate is subjected to gear turning and Ni back-gold treatment; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 90MPa, the temperature is 400 ℃, the heat preservation and pressure maintaining time is 3h, after welding processing, the sheath and the rare earth Gd target material have no reaction and diffusion pollution, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Example nine
Protecting the welding surface of the rare earth Gd target blank, and sputtering and plating a protective material TaN on other surfaces of the rare earth target blank; the back plate adopts copper alloy CuCr1, and the welding surface of the back plate is subjected to gear turning and Ni back-gold treatment; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 400 ℃, the heat preservation and pressure maintaining time is 3h, the sheath and the rare earth Gd target material have no reaction and diffusion pollution after welding processing, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Example ten
Protecting the welding surface of the rare earth Gd target blank, and sputtering and plating a protective material TaN on other surfaces of the rare earth target blank; the back plate adopts copper alloy CuCr1, and the welding surface of the back plate is subjected to gear turning and Ni back-gold treatment; processing a 6061Al sheath material by a common vehicle, cleaning the sheath material before welding, and coating BN on the inner surface of the sheath for protection treatment; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and performing HIP welding processing on the seal welding target material, wherein the HIP pressure is 110MPa, the temperature is 400 ℃, the heat preservation and pressure maintaining time is 3h, the sheath and the rare earth Gd target material have no reaction and diffusion pollution after welding processing, the sheath and the target material can be automatically separated, and the rare earth target material is effectively protected. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Comparative example 1
Turning teeth on the welding surface of the rare earth Y target blank; the back plate is made of copper alloy C18000, and the welding surface of the back plate is subjected to gear turning; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, and cleaning before welding; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 4h, after welding processing, a sheath and the rare earth Y target material are subjected to reaction and diffusion pollution, the sheath and the target material cannot be automatically separated, and the rare earth target material and the sheath cannot be subjected to protection treatment to prevent material reaction failure. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Comparative example No. two
The welding surface of the rare earth Y target blank is a plane; the back plate is made of copper alloy C18000, and the welding surface of the back plate is a plane; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, and cleaning before welding; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 4h, after welding processing, a sheath and the rare earth Y target material are subjected to reaction and diffusion pollution, the sheath and the target material cannot be automatically separated, and the rare earth target material and the sheath cannot be subjected to protection treatment to prevent material reaction failure. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Comparative example No. three
The welding surface of the rare earth Y target blank is a plane, and Ni back-gold treatment is carried out on the welding surface; the back plate is made of copper alloy C18000, the welding surface of the back plate is a plane, and Ni back-gold treatment is carried out on the welding surface; the intermediate layer is made of 1060Al material with the thickness of 2 mm; processing a 6061Al sheath material by a common vehicle, and cleaning before welding; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 4h, after welding processing, a sheath and the rare earth Y target material are subjected to reaction and diffusion pollution, the sheath and the target material cannot be automatically separated, and the rare earth target material and the sheath cannot be subjected to protection treatment to prevent material reaction failure. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
Comparative example No. four
The welding surface of the rare earth Y target blank is a plane; the back plate is made of copper alloy C18000, the welding surface of the back plate is a plane, and Ni back-gold treatment is carried out on the welding surface; no interlayer material; processing a 6061Al sheath material by a common vehicle, and cleaning before welding; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 300 ℃, the heat preservation and pressure maintaining time is 4h, after welding processing, a sheath and the rare earth Y target material are subjected to reaction and diffusion pollution, the sheath and the target material cannot be automatically separated, and the rare earth target material and the sheath cannot be subjected to protection treatment to prevent material reaction failure. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld ratio and weld strength data are shown in table 1, and the welded structure of the target without the intermediate layer is shown in fig. 8 and 9.
Comparative example five
Only carrying out Ni back-gold treatment on the welding surface of the rare earth Y target blank, wherein the welding surface of the target blank is a plane; the back plate is made of copper alloy C18000, and the welding surface of the back plate is a plane; and welding by adopting an In brazing mode, and performing 2-layer vacuum packaging protection after processing each rare earth material before welding. The weld joint rate and weld strength data are shown in table 1.
Comparative example six
The welding surface of the rare earth Gd target blank is a plane; the back plate adopts copper alloy CuCr1, and the welding surface of the back plate is turned with teeth; processing a 6061Al sheath material by a common vehicle, and cleaning before welding; assembling the rare earth target and the back plate in the sheath, and performing electron beam seal welding processing; and (3) carrying out HIP welding processing on the seal welding target material, wherein the HIP pressure is 100MPa, the temperature is 400 ℃, the heat preservation and pressure maintaining time is 3h, after welding processing, the sheath and the rare earth Gd target material are subjected to reaction and diffusion pollution, the sheath and the target material cannot be automatically separated, and the rare earth target material and the sheath cannot be subjected to protection treatment to prevent material reaction failure. Before welding, 2 layers of vacuum packaging protection are carried out after processing of each sequence of rare earth materials. The weld joint rate and weld strength data are shown in table 1.
TABLE 1 weld joint ratio and weld strength values in examples and comparative examples
As can be seen from table 1, in the examples and the comparative examples, the target welding rate is above 99%, the target welding strength in the examples is above 60MPa, and in the comparative examples one to six, the target welding strength is below 60MPa, which cannot meet the requirement of high welding strength, and it can be seen that the welding rate cannot completely represent the welding performance index; in the first comparative example, the fourth comparative example and the sixth comparative example, the rare earth target reacts and diffuses with the sheath, and the target scrapping risk is increased; the fifth comparative example is In brazing, and the welding strength is 5MPa, which is much lower than the diffusion welding strength In the examples.
Claims (10)
1. The welding method of the high-purity rare earth and alloy target is characterized by comprising the following steps of:
1) processing a rare earth target blank and a back plate: carrying out gear turning on the welding surfaces of the rare earth target blank and the back plate, carrying out back gold treatment on the gear turning surface, and then carrying out vacuum packaging;
2) surface treatment of the rare earth target blank: plating a protective layer on the non-welding surface of the rare earth target blank;
3) designing an intermediate layer: arranging an intermediate layer on a welding interface of the rare earth target blank and the back plate;
4) and (3) sheath processing: preparing a sheath for welding by a common vehicle, and cleaning the sheath before welding;
5) special treatment of sheathing: uniformly coating a protective layer on the inner surface of the sheath, and drying;
6) and (3) electron beam seal welding processing: assembling the rare earth target blank, the intermediate layer and the back plate into a sheath, and performing electron beam sealing welding processing on the sheath interface under a vacuum condition to obtain a sealing welding target material;
7) hot isostatic pressing diffusion welding processing: and (3) carrying out hot isostatic pressure diffusion welding processing on the seal welding target material, biting the turning tooth structures of the rare earth target blank and the back plate into the intermediate layer material, carrying out diffusion welding, and removing the sheath to obtain the integrated high-purity rare earth target material.
2. The method of claim 1, wherein the rare earth materials of the high purity rare earth target comprise: any one of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium metal, and alloys thereof; the back plate material comprises aluminum alloy, copper or copper alloy; the welding rate of the high-purity rare earth target material is more than or equal to 99 percent, and the welding strength is more than or equal to 60 MPa.
3. The method according to claim 1, wherein the protective layer material in step 5) is BN or ZrO2。
4. The method of claim 1, wherein the protective layer material in step 2) is TaN or TiN.
5. The method as claimed in claim 1, wherein the back gold method in step 1) adopts a magnetron sputtering coating method, and the sputtered film is a high-purity Ni or NiV film.
6. The method as claimed in claim 1, wherein the step 1) of turning the teeth structure is that V-shaped depressions and trapezoidal convex parts are distributed at intervals, the bottom angle alpha of the V-shaped depressions is 55 degrees, and two sides of the angle are symmetrical about a bisector of the bottom angle; the depth h of the V-shaped concave part and the trapezoidal convex part is 0.2 cm; the length L of every two adjacent V-shaped depressions and trapezoidal convex parts is 0.35 cm.
7. The method as claimed in claim 1, wherein the material of the intermediate layer in the step 3) is pure aluminum or titanium, and the thickness is 1.8-8 mm.
8. The method as claimed in claim 1, wherein 6061Al or stainless steel is adopted as the jacket material in the step 4), and the jacket is subjected to acid pickling treatment by using diluted hydrochloric acid to remove the surface oxide layer.
9. The method of claim 1, wherein the step 6) of electron beam sealing is performed in a vacuum environment.
10. The method as claimed in claim 1, wherein the welding temperature in step 7) is 250-600 ℃, the welding pressure is 80-120 MPa, and the heat preservation and pressure maintaining time is 2.5-5.5 h.
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