CN112658456A - Hot isostatic pressing integral forming method for target assembly - Google Patents
Hot isostatic pressing integral forming method for target assembly Download PDFInfo
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- CN112658456A CN112658456A CN202011471673.7A CN202011471673A CN112658456A CN 112658456 A CN112658456 A CN 112658456A CN 202011471673 A CN202011471673 A CN 202011471673A CN 112658456 A CN112658456 A CN 112658456A
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Abstract
The invention relates to the technical field of semiconductors, and provides a Hot Isostatic Pressing (HIP) integral forming method of a target assembly, which is characterized by comprising the following steps: providing a back plate, a target material and a vacuum sheath; sequentially placing the back plate and the target material into a vacuum jacket; placing the target on the backing plate; vacuumizing the vacuum sheath, and welding and sealing the vacuum sheath after the vacuum sheath reaches a preset vacuum degree; carrying out hot pressing treatment on the welded and sealed vacuum sheath by using a hot isostatic pressing process to obtain a target assembly integrally formed by the target and the back plate; and removing the vacuum sheath, and processing the target material assembly with the required size. In the embodiment of the invention, the welding problem of the target material and the back plate is solved through the integral forming process of the target material and the back plate, the target material and the back plate formed by the method can form a tight metallurgical bonding interface, the quality and the heat conductivity of a welding seam are ensured, and the forming and welding efficiency and the qualified rate of the chromium target material are greatly improved.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a Hot Isostatic Pressing (HIP) integral forming method for a target assembly.
Background
The sputtering technology is one of the common processes in the field of semiconductor manufacturing, and with the increasing development of the sputtering technology, the sputtering target plays an increasingly important role in the sputtering technology, and the quality of the sputtering target directly influences the film forming quality after sputtering. In the field of sputtering target manufacturing, a target assembly is composed of a target blank according with sputtering performance and a back plate combined with the target blank through welding.
When the target assembly is prepared by the prior art method, a target prepared in advance is generally welded with a back plate. Because the target material can be oxidized even at normal temperature, a compact oxide film can be generated on the surface, and the welding strength is lower, the efficiency is low, even the welding can not be carried out by the existing welding mode, so that the product percent of pass is lower.
Disclosure of Invention
The embodiment of the invention provides a hot isostatic pressing integral forming method for a target assembly, which can reduce the phenomenon that a target is oxidized during welding, improve the welding strength of the target and a back plate and improve the product yield. The specific scheme is as follows:
the embodiment of the invention provides a hot isostatic pressing integral forming method of a target assembly, which comprises the following steps:
providing a back plate, a target material and a vacuum sheath;
sequentially placing the back plate and the target material into a vacuum jacket;
placing the target on the backing plate;
vacuumizing the vacuum sheath, and welding and sealing the vacuum sheath after the vacuum sheath reaches a preset vacuum degree;
carrying out hot pressing treatment on the welded and sealed vacuum sheath by using a hot isostatic pressing process to obtain a target assembly integrally formed by the target and the back plate;
and removing the vacuum sheath, and processing the target material assembly with the required size.
Optionally, before the back plate and the target are sequentially placed in the vacuum envelope, the method further includes the following steps:
providing an intermediate layer, and putting the intermediate layer into a vacuum envelope;
the placing the target on the backing plate comprises:
placing the intermediate layer on a back plate, wherein the roughness of the surface of the intermediate layer, which is in contact with the back plate, and the roughness of the surface of the back plate, which is in contact with the intermediate layer are both smaller than a preset roughness value;
and placing the target material on the intermediate layer, wherein the roughness of the surface of the intermediate layer, which is in contact with the target material, and the roughness of the surface of the target material, which is in contact with the intermediate layer are both smaller than the preset roughness value, and the intermediate layer is positioned between the target material and the back plate.
Optionally, before the placing the target on the backing plate, the method further comprises:
cleaning the back plate, the intermediate layer, the target material and the vacuum sheath, wherein the thickness of the intermediate layer is less than or equal to 0.3 mm;
the vacuum sheath is made of stainless steel materials, and the wall thickness range of the vacuum sheath is 1.5mm-3.5 mm;
or the vacuum sheath material is a glass material, and the wall thickness range of the vacuum sheath is 2mm-5 mm.
Optionally, the back plate is a copper back plate, the target material is a chromium target material, the chromium target material is spherical powder of 50-230 meshes, and the oxygen content of the target material is less than or equal to 1000 million parts per million (ppm).
Optionally, the evacuating the vacuum jacket includes:
vacuumizing the vacuum sheath at normal temperature;
vacuumizing the vacuum sheath in a temperature environment with the temperature higher than the preset temperature;
the welding method for welding the vacuum sheath is gas shielded welding.
Optionally, the vacuum sheath is processed at normal temperatureWhen vacuumizing, the vacuumizing time is more than or equal to 1 hour, and the vacuum degree is required to be at least 10-2Megapascals (MPa).
Optionally, when the vacuum sheath is vacuumized in the temperature environment with the temperature higher than the preset temperature, the preset temperature is 200 ℃, the vacuumizing time is not less than 3 hours, and the vacuum degree is required to be at least 10-2Megapascals (MPa).
Optionally, the hot isostatic pressing process comprises: and (3) placing the vacuum sheath after vacuumizing in an environment of 430-520 ℃, simultaneously applying pressure of 90-140 MPa, keeping for 1-4 hours, then relieving pressure, cooling to below 200 ℃, and discharging.
Optionally, the hot isostatic pressing process is carried out at a temperature of 880-950 ℃ and a pressure of 90-150 MPa for 1-4 hours.
Optionally, the vacuum sheath is removed by machining or electrochemical corrosion, and the target assembly with the required size is machined by a machining method.
In the embodiment of the invention, the welding problem of the target material and the back plate is solved through the integral forming process of the target material and the back plate, the target material and the back plate formed by the method can form a compact metallurgical bonding section, the quality and the heat conductivity of a welding seam are ensured, and the forming and welding efficiency and the qualified rate of the chromium target material are greatly improved. By strictly controlling the quality of the chromium target and meeting the requirement on the vacuum degree of a vacuum sheath, the uniformity of components of the formed chromium target is ensured, and the problem of oxidation of the welding surface of the chromium target and a copper back plate is avoided. In addition, the hot isostatic pressing process realizes metallurgical bonding of the welding section between the target and the back plate, the surface of the bonding part has atom interdiffusion with a certain depth, and the bonding strength is high. Meanwhile, the target material can be ensured to have fine and uniform grain size due to low forming temperature.
Drawings
FIG. 1 is a schematic flow diagram of a hot isostatic pressing bulk forming method for a target assembly according to an embodiment of the invention;
fig. 2 is a schematic structural diagram of the arrangement of components in a vacuum sheath in the process of manufacturing a target assembly by the hot isostatic pressing bulk forming method for the target assembly according to the embodiment of the invention. she
Detailed Description
The technical solutions in the embodiments of the present invention will be described below with reference to the drawings in the embodiments of the present invention. In the description of the embodiments of the present invention, where "/" denotes an or meaning, for example, a/B may denote a or B; "and/or" herein is merely an association describing an associated object, and means that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, in the description of the embodiments of the present invention, "a plurality" means two or more than two.
In the following, the terms "first", "second" and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", "third" may explicitly or implicitly include one or more of the features.
The invention provides a hot isostatic pressing integral forming method of a target assembly, which can reduce the phenomenon that a target is oxidized during welding, improve the welding strength of the target and a back plate and improve the product percent of pass.
As shown in fig. 1, a hot isostatic pressing bulk forming method for a target assembly according to an embodiment of the present invention includes the following steps:
s1: providing a back plate, a target material and a vacuum sheath;
s2: sequentially placing the back plate and the target material into a vacuum jacket;
s3: placing the target on the backing plate;
s4: vacuumizing the vacuum sheath, and welding and sealing the vacuum sheath after the vacuum sheath reaches a preset vacuum degree;
s5: carrying out hot pressing treatment on the welded and sealed vacuum sheath by using a hot isostatic pressing process to obtain a target assembly integrally formed by the target and the back plate;
s6: and removing the vacuum sheath, and processing the target material assembly with the required size.
In the embodiment of the invention, the hot isostatic pressing process realizes metallurgical bonding of the welding section between the target material and the back plate, the surface of the bonding part has atom interdiffusion with a certain depth, the bonding strength is high, the target material and the back plate can be tightly jointed and formed, and the problem of welding the target material and the back plate is solved.
Optionally, after the back is placed in the vacuum sheath, the back plate can be attached to the inner bottom surface of the vacuum sheath and fixed and positioned by the positioning pins.
Optionally, before the back plate and the target are sequentially placed in the vacuum envelope, the method further includes the following steps:
providing an intermediate layer, and putting the intermediate layer into a vacuum envelope;
the placing the target on the backing plate comprises:
placing the intermediate layer on a back plate, wherein the roughness of the surface of the intermediate layer, which is in contact with the back plate, and the roughness of the surface of the back plate, which is in contact with the intermediate layer are both smaller than a preset roughness value;
and placing the target material on the intermediate layer, wherein the roughness of the surface of the intermediate layer, which is in contact with the target material, and the roughness of the surface of the target material, which is in contact with the intermediate layer are both smaller than the preset roughness value, and the intermediate layer is positioned between the target material and the back plate.
The predetermined roughness value may be a degree of 6.4 um.
Optionally, before the placing the target on the backing plate, the method further comprises:
cleaning the back plate, the intermediate layer, the target material and the vacuum sheath, wherein the thickness of the intermediate layer is less than or equal to 0.3 mm;
the vacuum sheath is made of stainless steel materials, and the wall thickness range of the vacuum sheath is 1.5mm-3.5 mm;
or the vacuum sheath material is a glass material, and the wall thickness range of the vacuum sheath is 2mm-5 mm.
Optionally, the back plate, the intermediate layer, the target material and the vacuum sheath may be soaked and cleaned with an alcohol or acetone solution. Optionally, the intermediate layer may be a titanium material with a thickness of 0.2-0.8 mm.
Optionally, the back plate is a copper back plate, the target material is a chromium target material, the chromium target material is spherical powder of 50-230 meshes, and the oxygen content of the target material is less than or equal to 1000 million parts per million (ppm).
Optionally, the evacuating the vacuum jacket includes:
vacuumizing the vacuum sheath at normal temperature;
vacuumizing the vacuum sheath in a temperature environment with the temperature higher than the preset temperature;
the welding method for welding the vacuum sheath is gas shielded welding. For example, the Welding method for Welding the vacuum jacket may be non-melting Inert Gas Tungsten Welding (TIG) Welding or metal Inert-Gas Welding (MIG) Welding.
Optionally, when the vacuum sheath is vacuumized at normal temperature, the vacuumizing time is more than or equal to 1 hour, and the required vacuum degree is at least 10-2Megapascals (MPa).
Optionally, when the vacuum sheath is vacuumized in the temperature environment with the temperature higher than the preset temperature, the preset temperature is 200 ℃, the vacuumizing time is not less than 3 hours, and the vacuum degree is required to be at least 10-2Megapascals (MPa).
Optionally, the hot isostatic pressing process comprises: and (3) placing the vacuum sheath after vacuumizing in an environment of 430-520 ℃, simultaneously applying pressure of 90-140 MPa, keeping for 1-4 hours, then relieving pressure, cooling to below 200 ℃, and discharging.
Optionally, the hot isostatic pressing process is carried out at a temperature of 880-950 ℃ and a pressure of 90-150 MPa for 1-4 hours.
Optionally, the vacuum sheath is removed by machining or electrochemical corrosion, and the target assembly with the required size is machined by a machining method.
In the embodiment of the invention, after the back plate, the target material and the intermediate layer are placed in the vacuum sheath, the back plate, the intermediate layer and the target material are ensured to be in close contact, and then the vacuum welding and sealing are carried out.
In the invention, the vacuum bag which is sealed and welded can be placed in a hot isostatic pressing device for hot isostatic pressing treatment.
Optionally, the process of welding, sealing and vacuumizing before the hot isostatic pressing treatment of the vacuum sheath may specifically be: after chromium particles are filled, vacuumizing the vacuum sheath for 1-5h at normal temperature, and ensuring that the vacuum degree is at least 10-2 Pa; placing the vacuum sheath in an environment of 100-350 ℃ for vacuumizing for 2-6h, and ensuring that the vacuum degree is at least 10-2 Pa; and then welding and sealing the vacuum sheath.
Specifically, as shown in fig. 2, a chromium target 4, an intermediate layer 5, a copper backing plate 6, and a steel can 3 may be provided.
The purity of the chromium target 4 is more than or equal to 99.999 percent, the oxygen content is less than or equal to 1000ppm, the chromium target is in a shape of a round cake, and the thickness is 50 mm; according to the actual application requirement, the shape of the outer surface can be other regular shapes or special-shaped pieces such as a cylinder, a hexahedron and the like, the implementation process is cylindrical, and the surface precision of the combined surface of the middle layer 5 and the outer surface is 3.2.
The middle layer 5 is a titanium foil with the thickness of 0.3mm, the shape and the size of the middle layer are determined according to the chromium target material, the middle layer is flatly paved on the connecting surface of the chromium target material and the copper back plate, and the middle layer has the function of ensuring the connecting quality of the welding interface of the chromium target material and the copper back plate.
The copper back plate 6 is an oxygen-free copper or chromium-containing copper alloy back plate, the size and the shape of the copper back plate are close to those of the chromium target 4, the middle groove is the shape of the formed chromium target, and the surface precision of the combination surface of the copper back plate and the middle layer 5 is 3.2. And the chromium target 4 is placed on a copper back plate 6, and a titanium foil 5 is flatly paved in the middle.
The steel sheath 3 is made of stainless steel or carbon steel, the size and the shape of the steel sheath are the same as those of the copper back plate 6, and the wall thickness is 3 mm. And after the chromium target 4, the intermediate layer 5 and the copper back plate 6 are arranged in the inner cavity of the steel sheath 3, welding the sheath 3, and then vacuumizing.
Referring to fig. 2, one end of the vacuum degassing pipe 1 is connected with the upper end cover of the steel sheath 3, and the other end is connected with the degassing pump 2. The vacuumizing process comprises the steps of vacuumizing for more than or equal to 3 hours at normal temperature, then vacuumizing for more than or equal to 3 hours by placing the steel sheath 3 in an environment with the temperature of 200 ℃, then heating to the temperature of less than or equal to 400 ℃, vacuumizing for more than or equal to 2 hours, and sealing and welding the steel sheath 3 after vacuumizing is finished.
The steel can 3 can be placed in a HIP process shown in a hot isostatic pressing device, and the HIP process parameters are as follows: the pressure is more than or equal to 100MPa, the temperature is more than or equal to 900 ℃, and the time is more than or equal to 2 h.
And taking out the steel sheath 3 after the hot isostatic pressing is finished, machining to remove the steel sheath 3 outside to obtain a target assembly formed by combining the chromium target 4 and the copper back plate 6, and machining the outer ring connecting thread of the copper back plate 6 to obtain the required chromium-copper target integral forming assembly.
It should be understood that the above description is only for the purpose of facilitating a better understanding of the embodiments of the present invention by those skilled in the art, and is not intended to limit the scope of the embodiments of the present invention. Various equivalent modifications or changes, or combinations of any two or more of the above, may be apparent to those skilled in the art in light of the above examples given. Such modifications, variations, or combinations are also within the scope of the embodiments of the invention.
It should also be understood that the foregoing descriptions of the embodiments of the present invention focus on highlighting differences between the various embodiments, and that the same or similar parts that are not mentioned may be referred to one another, and thus, for brevity, will not be described again.
It should also be understood that the manner, case, category and division of the embodiments of the present invention are only for convenience of description and should not be construed as a particular limitation, and features in various manners, cases and embodiments may be combined without contradiction.
It is also to be understood that the terminology and/or the description of the various embodiments are consistent and mutually exclusive, and that features of different embodiments may be combined to form new embodiments according to their inherent logical relationships, unless otherwise specified or logically conflicting, in various embodiments of the present invention.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of changes or substitutions within the technical scope of the present invention, and all such changes or substitutions are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A Hot Isostatic Pressing (HIP) integral forming method of a target assembly is characterized by comprising the following steps:
providing a back plate, a target material and a vacuum sheath;
sequentially placing the back plate and the target material into a vacuum jacket;
placing the target on the backing plate;
vacuumizing the vacuum sheath, and welding and sealing the vacuum sheath after the vacuum sheath reaches a preset vacuum degree;
carrying out hot pressing treatment on the welded and sealed vacuum sheath by using a hot isostatic pressing process to obtain a target assembly integrally formed by the target and the back plate;
and removing the vacuum sheath, and processing the target material assembly with the required size.
2. The method of claim 1, wherein prior to sequentially placing the backing plate and the target into a vacuum envelope, the method further comprises:
providing an intermediate layer, and putting the intermediate layer into a vacuum envelope;
the placing the target on the backing plate comprises:
placing the intermediate layer on a back plate, wherein the roughness of the surface of the intermediate layer, which is in contact with the back plate, and the roughness of the surface of the back plate, which is in contact with the intermediate layer are both smaller than a preset roughness value;
and placing the target material on the intermediate layer, wherein the roughness of the surface of the intermediate layer, which is in contact with the target material, and the roughness of the surface of the target material, which is in contact with the intermediate layer are both smaller than the preset roughness value, and the intermediate layer is positioned between the target material and the back plate.
3. The method of claim 2, wherein prior to said placing said target on said backing plate, said method further comprises:
cleaning the back plate, the intermediate layer, the target material and the vacuum sheath, wherein the thickness of the intermediate layer is less than or equal to 0.3 mm;
the vacuum sheath is made of stainless steel materials, and the wall thickness range of the vacuum sheath is 1.5mm-3.5 mm;
or the vacuum sheath material is a glass material, and the wall thickness range of the vacuum sheath is 2mm-5 mm.
4. The hot isostatic pressing bulk forming method for the target assembly according to claim 1, wherein the backing plate is a copper backing plate, the target is a chromium target, the chromium target is 50-230 mesh spherical powder, and the oxygen content of the target is less than or equal to 1000 parts per million (ppm).
5. The method for hot isostatic pressing of a target assembly according to claim 1, wherein said evacuating the vacuum capsule comprises:
vacuumizing the vacuum sheath at normal temperature;
vacuumizing the vacuum sheath in a temperature environment with the temperature higher than the preset temperature;
the welding method for welding the vacuum sheath is gas shielded welding.
6. The Hot Isostatic Pressing (HIP) bulk forming method of the target assembly according to claim 5, wherein when the vacuum sheath is vacuumized at normal temperature, the vacuuming time is not less than 1 hour, and the vacuum degree is required to be at least 10-2Megapascals (MPa).
7. The hot isostatic pressing integrated forming method for the target assembly according to claim 5, wherein when the vacuum sheath is vacuumized in an environment with a temperature higher than a preset temperature, the preset temperature is 200 ℃, the vacuuming time is not less than 3 hours, and the vacuum degree is required to be at least 10-2Megapascals (MPa).
8. The method of claim 1, wherein the hot isostatic pressing process comprises: and (3) placing the vacuum sheath after vacuumizing in an environment of 430-520 ℃, simultaneously applying pressure of 90-140 MPa, keeping for 1-4 hours, then relieving pressure, cooling to below 200 ℃, and discharging.
9. The method for hot isostatic pressing bulk forming of a target assembly according to claim 1, wherein the hot isostatic pressing process is carried out at a temperature ranging from 880 ℃ to 950 ℃ and at a pressure ranging from 90MPa to 150MPa for a period of time ranging from 1 hour to 4 hours.
10. The method of claim 1, wherein the vacuum sheath is removed by machining or electro-chemical etching, and the target assembly is machined to a desired size.
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