CN115354285B - Neutron target based on in-situ growth and preparation method thereof - Google Patents
Neutron target based on in-situ growth and preparation method thereof Download PDFInfo
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- CN115354285B CN115354285B CN202210897639.9A CN202210897639A CN115354285B CN 115354285 B CN115354285 B CN 115354285B CN 202210897639 A CN202210897639 A CN 202210897639A CN 115354285 B CN115354285 B CN 115354285B
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- 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
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- 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
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- 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
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- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- 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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
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Abstract
The invention relates to the technical field of accelerator type neutron targets, in particular to a neutron target based on in-situ growth and a preparation method thereof. One side of the substrate of the neutron target is provided with a plurality of pits; a hydrogen storage isotope layer and a sputtering resistant layer are sequentially arranged on one side surface of the substrate; the hydrogen storage isotope layer and the sputtering-resistant layer are recessed towards the substrate at the positions of the pits, so that the surface of the sputtering-resistant layer is provided with a plurality of sputtering pit pits. The preparation method comprises the steps of firstly processing a plurality of pits on one side of a substrate; and sequentially preparing a hydrogen storage isotope layer and a sputtering-resistant layer on one side of the substrate in an in-situ growth mode, so that the hydrogen storage isotope layer forms a structure identical to the pit, and a plurality of sputtering trap pits are formed on the surface of the sputtering-resistant layer. Atoms sputtered and flown out from the surface of the neutron target can be blocked by the inner wall of the sputtering well pit and redeposited in the sputtering well pit, so that the service life of the neutron target is greatly prolonged; the preparation method can keep the pit structure on the substrate and improve the comprehensive mechanical property of the neutron target.
Description
Technical Field
The invention relates to the technical field of accelerator type neutron targets, in particular to a neutron target based on in-situ growth and a preparation method thereof.
Background
Neutron technology is widely applied to fields such as neutron photography, oilfield logging, cancer treatment, neutron security inspection, activation analysis, irradiation breeding, irradiation damage research, nuclear measurement and the like. Currently the main neutron sources are nuclear reactors, radioactive sources and accelerator type neutron sources. The accelerator type deuterium-tritium neutron source bombards a neutron target through an accelerated deuterium ion beam, and generates a fusion neutron of 14.1MeV through a deuterium-tritium fusion reaction. The accelerator type deuterium-tritium neutron source can generate neutrons only by electrifying, so that the safety is high. In addition, the neutron source has the advantages of miniaturization, portability, low cost and the like, and has wide application prospect.
In deuterium-deuterium fusion neutron generators, the neutron target is the core component that directly generates neutrons. Wherein the lifetime of the neutron target is critical to the operating and use costs of the neutron generator. Neutron targets commonly used at present are mainly divided into prefabricated targets and self-forming targets. The prefabricated target is generally a single titanium film plated on a substrate, deuterium/tritium is obtained by absorbing deuterium/tritium through the titanium film, the deuterium/tritium titanium target is placed in an accelerator, and the deuterium/tritium titanium target is bombarded by a deuterium ion beam to generate neutrons through fusion reaction; a single titanium film is plated on a substrate from a target to form a titanium target, the titanium target is directly arranged in an accelerator, an accelerated deuterium ion beam bombards the titanium target and deposits the titanium target in the operation process, and then the deuterium ion beam bombarding the titanium target and deuterium deposited in the titanium target generate fusion reaction to generate neutrons. In any neutron target, the neutron target is bombarded by a high-speed deuterium ion beam in the operation process, and the titanium film has a sputtering effect under the bombardment of the high-energy ion beam. That is, when the high-speed deuterium ion beam bombards the surface of the neutron target, the kinetic energy and momentum of deuterium ions are transferred to atoms on the surface of the neutron target, so that the surface atoms are splashed and lost due to the rupture of chemical bonds. Due to the sputtering effect caused by the special operating environment, the neutron target film is continuously sputtered and thinned until the neutron target film is invalid, and the operating life of the neutron target is greatly reduced. Therefore, how to effectively reduce the sputtering effect of the neutron target is one of key technologies for prolonging the service life of the neutron target.
Since the sputtering effect is closely related to the kind of material. The current method for improving the sputtering resistance of the neutron target is to prepare a layer of material with low sputtering rate on the surface of the neutron target film as a sputtering resistant film. However, the size of the sputter-resistant film cannot be too thick. The reason is that the high-energy deuterium ion beam can not penetrate through the sputtering-resistant film to reach the hydrogen storage isotope layer (titanium film layer) to generate neutrons through fusion reaction, or the number of deuterium atoms which can reach the hydrogen storage isotope layer and deuterium/tritium atoms in the hydrogen storage isotope layer is reduced due to the blocking effect of the sputtering-resistant film, so that the neutron yield is reduced, and the use requirement is not met. The thickness of the sputter-resistant film is thus typically in the order of nanometers. Because the sputter-resistant film is too thin, it is sputtered off quickly, leaving a bare hydrogen storage isotope layer (titanium film layer), although the sputtering rate is low. Therefore, the sputtering-resistant film prepared by the traditional method has extremely limited effect of improving the service life of the neutron target, and can not meet the use requirement of the long-life neutron target.
Therefore, how to solve the problem of sputtering resistance of the neutron target, thereby greatly improving the service life of the neutron target is a technical bottleneck to be solved urgently.
Disclosure of Invention
The invention aims to provide a neutron target based on in-situ growth and a preparation method thereof.
The technical scheme for solving the technical problems is as follows:
the invention provides a neutron target based on in-situ growth, which comprises a substrate, wherein one side of the substrate is provided with a plurality of pits; a hydrogen storage isotope layer and a sputtering resistant layer are sequentially arranged on one side surface of the substrate; the hydrogen storage isotope layer and the sputtering-resistant layer are recessed towards the substrate at positions corresponding to the pits, so that the surface of the sputtering-resistant layer is provided with a plurality of sputtering pit pits.
On the basis of the technical scheme, the invention can be improved as follows.
Furthermore, the pit of the sputtering well is in an inverted conical shape, and the relation between the diameter D of the large end and the depth h is D/h more than or equal to 0.38.
Further, the relation between the distance a between the centers of the large end circles of the adjacent sputtering well pits and the large end diameter D is that
Further, the value of the large end diameter D is 0.2-2 mm.
Further, the material of the sputtering-resistant layer comprises one or more of ceramics, tungsten alloy, palladium alloy, tantalum alloy and nickel alloy, and the thickness range of the sputtering-resistant layer is 100-500nm;
the material of the hydrogen storage isotope layer comprises one or more of titanium, nickel, zirconium, magnesium, molybdenum, aluminum, vanadium, tantalum and rare earth elements, and the thickness of the hydrogen storage isotope layer is 0.5-5 mu m;
the substrate is made of copper, copper alloy, silver alloy, molybdenum or molybdenum alloy.
The invention also provides a neutron target preparation method based on in-situ growth, which comprises the following steps:
s1, processing a plurality of pits on one side of the substrate;
s2, preparing a hydrogen storage isotope layer and a sputtering-resistant layer on one side of the substrate in sequence in an in-situ growth mode, enabling the hydrogen storage isotope layer to form a structure identical to the pit, and enabling the surface of the sputtering-resistant layer to form a plurality of sputtering well pits.
Further, before step S1, polishing the surface of one side of the substrate to have a roughness of 0.1-3.2 μm, and then sequentially cleaning the surface of the substrate with acetone, ethanol and deionized water for 15-30min each time.
Further, in the step S1, a manner of processing the plurality of pits is surface extrusion molding; the extrusion pressure is 5-20MPa greater than the yield strength of the material of the substrate, and the extrusion pressure is kept for 1-10min.
Further, in the step S2, the in-situ growth mode is a magnetron sputtering method; the method comprises the following steps:
coating a film on one side of the substrate by using corresponding materials in sequence in an inert gas environment by using magnetron sputtering equipment, and obtaining the hydrogen storage isotope layer and the sputtering resistant layer; wherein, the coating pressure is less than 10Pa, and the power is less than 500W.
Further, after the step S2 is finished, the method further includes a step S3:
s3, performing in-situ heat treatment to enable the substrate and the hydrogen storage isotope layer to diffuse mutually at the interface between the substrate and the hydrogen storage isotope layer, and forming a solid solution transition layer;
the in-situ heat treatment is high-temperature diffusion treatment, and the high-temperature diffusion treatment is carried out under vacuum degree of less than 10 -4 And the high-temperature diffusion treatment is carried out under the condition of Pa, wherein the temperature of the high-temperature diffusion treatment is 500+/-50 ℃ and the time is 500+/-20 min.
The invention has the beneficial effects that:
(1) According to the neutron target based on in-situ growth, the plurality of sputtering trap pits are formed in the surface of the sputtering-resistant layer, so that atoms sputtered from the surface of the neutron target can be blocked by the inner wall of the sputtering trap pits and redeposited in the sputtering trap pits, and therefore, the atoms cannot be separated from the surface of the material of the sputtering-resistant layer, the sputtering rate of the material of the sputtering-resistant layer is greatly reduced, and the service life of the neutron target is greatly prolonged;
(2) According to the neutron target based on in-situ growth, the sputtering trap pits are obtained by in-situ growth on the pits of the substrate, and the pits are not simply arranged on the surface of the sputtering-resistant layer, so that the sputtering-resistant layer is kept at a uniform thickness, and the service life of the neutron target is ensured;
(3) According to the neutron target based on in-situ growth, the substrate, the hydrogen storage isotope layer and the sputtering-resistant layer are mutually meshed through the pit structure, so that the neutron target has stronger interface binding force compared with the planar connection of all layers of a common neutron target, and the falling and separation conditions under the action of strong stress are effectively prevented;
(4) Compared with the common neutron target, the service life of the neutron target based on in-situ growth can be prolonged by 200-300%;
(5) According to the neutron target preparation method based on in-situ growth, the pit is firstly processed on the substrate in an in-situ growth mode, and then the hydrogen storage isotope layer and the sputtering-resistant layer are prepared, so that the pit structure on the substrate can be reserved, the influence on the interface bonding strength of the film layer when the sputtering pit is manufactured later is effectively avoided, and the comprehensive mechanical property of the neutron target is improved;
(6) According to the neutron target preparation method based on in-situ growth, after the hydrogen storage isotope layer and the sputtering-resistant layer are prepared, in-situ heat treatment is carried out, so that the substrate and the hydrogen storage isotope layer and the sputtering-resistant layer are mutually diffused, a solid solution transition layer is formed, and the interface binding force between the layers is further improved while the layers are mutually meshed through the pit structure;
(7) The neutron target preparation method based on in-situ growth has the advantages of simple steps, high efficiency and low cost, and can be suitable for preparing neutron targets of various materials.
Drawings
FIG. 1 is a cross-sectional structural view of an in-situ growth-based neutron target of the invention;
fig. 2 is a front view of a sputter-resistant layer and sputter trap pits of the in-situ grown neutron target of the invention.
In the drawings, the list of components represented by the various numbers is as follows:
1. a sputter-resistant layer; 2. sputtering pit; 3. a hydrogen storage isotope layer; 4. a substrate.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
As shown in fig. 1 and 2, the neutron target based on in-situ growth of the invention comprises a substrate 4, wherein one side of the substrate 4 is provided with a plurality of pits; the surface of one side of the substrate 4 is sequentially provided with a hydrogen storage isotope layer 3 and a sputtering-resistant layer 1, and the hydrogen storage isotope layer 3 and the sputtering-resistant layer 1 are recessed towards the substrate 4 at positions corresponding to the plurality of pits, so that the surface of the sputtering-resistant layer 1 is provided with a plurality of sputtering pit pits 2.
According to the neutron target based on in-situ growth, the surface of the sputtering-resistant layer 1 is provided with the plurality of sputtering trap pits 2, and when the neutron target is used, high-speed deuterium ion beams bombard the surface of the neutron target through the sputtering trap effect, atoms on the surface of the neutron target are sputtered, and the sputtered atoms are blocked by the inner wall of the sputtering trap pits 2 and are redeposited in the sputtering trap pits 2, so that the sputtered atoms cannot be separated from the surface of the material of the sputtering-resistant layer 1, the sputtering rate of the material of the sputtering-resistant layer 1 is greatly reduced, the sputtering rate of the neutron target from the source is effectively reduced, and the service life of the neutron target is greatly prolonged.
In addition, if the sputter-resistant layer 1 is thinned, it will be sputtered off quickly, exposing the underlying hydrogen storage isotope layer 3, greatly limiting the life of the neutron target. The sputtering well pit 2 is formed on the pit of the substrate 4, and the pit is not simply arranged on the surface of the sputtering-resistant layer 1, so that the sputtering-resistant layer 1 can keep uniform thickness, and the service life of a neutron target can be ensured.
Meanwhile, the neutron target provided by the invention has stronger interface binding force compared with the plane connection between layers of a common neutron target by mutually occluding the substrate 4, the hydrogen storage isotope layer 3 and the sputtering-resistant layer 1 through the pit structure, and effectively prevents the falling and separation under the action of strong stress.
The hydrogen storage isotope layer 3 may specifically be a deuterium storage layer, a tritium storage layer or a mixture layer of deuterium and tritium storage.
Preferably, the plurality of sputter well pits 2 of the present invention are uniformly arranged in a matrix form.
Preferably, the sputtering well pit 2 is in an inverted conical shape, and the relation between the large end diameter D and the depth h is D/h more than or equal to 0.38; the conical sputtering well pit 2 can block the atoms sputtered in the sputtering well pit 2 to the maximum extent, and if the bottom of the sputtering well pit 2 is arranged to be flat, the atoms at the position can be easily escaped.
Preferably, the relation between the distance a between the centers of the large ends of the adjacent sputtering well pits 2 and the diameter D of the large ends is thatIf the arrangement of the sputtering well pits 2 is too dense, the material in the areas of the non-sputtering well pits 2 can be sputtered off, thereby affecting the service life of the neutron target; if the arrangement of the sputtering pit 2 is too sparse, the effect of the sputtering pit is affected, the overall sputtering resistance is reduced, and the requirements cannot be met.
Preferably, the diameter D of the large end of the sputter well pit 2 has a value of 0.2 to 2mm.
Preferably, the material of the sputtering-resistant layer 1 comprises one or more of ceramics, tungsten alloy, palladium alloy, tantalum alloy and nickel alloy, and the thickness of the sputtering-resistant layer 1 ranges from 100 nm to 500nm.
Preferably, the material of the hydrogen storage isotope layer 3 comprises one or more of titanium, nickel, zirconium, magnesium, molybdenum, aluminum, vanadium, tantalum and rare earth elements, and the thickness of the hydrogen storage isotope layer 3 is 0.5-5 μm.
Preferably, the material of the substrate 4 is copper, copper alloy, silver alloy, molybdenum or molybdenum alloy.
According to the neutron target preparation method based on in-situ growth, a plurality of pits are processed on one side of the substrate 4, and then the hydrogen storage isotope layer 3 and the sputtering-resistant layer 1 are sequentially prepared on one side of the substrate 4 in an in-situ growth mode, so that the hydrogen storage isotope layer 3 has the same structure as the pits, and a plurality of sputtering trap pits 2 are formed on the surface of the sputtering-resistant layer 1.
If the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 are prepared on the substrate 4, and then the sputtering well pit 2 is prepared, in the preparation process of the sputtering well pit 2, the bonding interfaces of the substrate 4, the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 are damaged, and even the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 are broken and fall off, so that the preparation is failed.
According to the preparation method, the pit is firstly processed on the substrate 4 in an in-situ growth mode, then the hydrogen storage isotope layer 3 and the sputtering-resistant layer 1 are prepared, so that the pit structure on the substrate 4 can be reserved, and finally the sputtering-resistant layer 1 with the sputtering pit 2 structure is prepared, the influence on the interface bonding strength of the film layer when the sputtering pit 2 is manufactured later is effectively avoided, and the comprehensive mechanical property of the neutron target is improved.
Preferably, the substrate 4 is processed into a plurality of pits by surface etching, 3D printing or surface extrusion.
Preferably, the in-situ growth mode is a magnetron sputtering method, a thermal vacuum evaporation method, a pulse laser method or chemical vapor deposition method.
Preferably, the preparation method of the invention comprises the following steps:
1) Polishing the surface of the substrate 4 to a roughness of 0.1-3.2 mu m, and then sequentially cleaning the surface of the substrate by adopting acetone, ethanol and deionized water, wherein the cleaning time is respectively 15-30min each time.
2) Extruding one side surface of the substrate 4 by adopting a conical boss die, and processing a plurality of pits; wherein the extrusion pressure is 5-20MPa higher than the material yield strength of the substrate 4, and the pressure is maintained for 1-10min.
3) Sequentially preparing the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 on one side of the substrate 4 by using magnetron sputtering equipment; each preparation is carried out in an inert gas environment, the coating pressure of the magnetron sputtering equipment is less than 10Pa, and the power is less than 500W.
4) And performing in-situ heat treatment in a magnetron sputtering device, performing high-temperature diffusion treatment to diffuse the substrate 4 and the hydrogen storage isotope layer 3 to each other at the interface between the substrate and the hydrogen storage isotope layer, and forming a solid solution transition layer.
Wherein the high-temperature diffusion treatment temperature is 500+ -50deg.C, the time is 500+ -20 min, and the vacuum degree is less than 10 -4 Pa; the thickness of the solid solution transition layer is 0.3-1 mu m. And after the in-situ heat treatment is finished, obtaining the neutron target.
In the preparation method, after the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 are prepared, in-situ heat treatment is carried out, so that the substrate 4 and the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 are mutually diffused, a solid solution transition layer is formed, and the interface binding force between the layers is further improved while the layers are mutually meshed through the pit structure.
Since the sputtering-resistant layer 1 is thin, it is theoretically possible to form a transition layer with the hydrogen storage isotope layer 3, but the transition layer is thin and negligible.
The following is an illustration of the technical solution of the present invention by means of specific examples:
example 1
In the neutron target of the present embodiment, the material of the substrate 4 is CrZrCu alloy.
The hydrogen storage isotope layer 3 is a deuterium storage layer, the material of the hydrogen storage isotope layer is Ti55Mo45 alloy, the Ti55Mo45 alloy is smelted and molded according to the design proportion by adopting a vacuum smelting method, cast ingots are rolled, and the hydrogen storage isotope layer is processed into the target material size suitable for magnetron sputtering.
The material of the sputtering-resistant layer 1 is pure Pd.
The neutron target in this embodiment is prepared by plating the deuterium storage layer 3 and the sputtering resistant layer 1 on the surface of the substrate 4 in sequence, and the specific preparation process is as follows:
1) And (3) carrying out rough grinding and fine grinding on the surface of the CrZrCu substrate 4 to ensure that the roughness of the surface of the substrate 4 is less than 3.2 mu m, and then adopting acetone, ethanol and deionized water to clean sequentially, wherein the cleaning time is respectively 15-30min each time.
2) And extruding the surface of the substrate 4 by using a prefabricated conical boss die, wherein the extruding pressure is 340MPa, and the pressure is maintained for 5min. The specific dimensions of the pit obtained are as follows: the pits have a diameter of 0.8mm and a depth of 0.4mm, and are arranged at a distance of 1.5 mm.
3) After the surface treatment of the substrate 4 is finished, a deuterium storage layer and a sputtering resistant layer 1 are plated on the surface of the substrate 4 in sequence under the protection of Ar (99.999%) by adopting a magnetron sputtering method, the plating pressure is less than 1Pa, the plating power is less than 200W, the plating time is 30-240min, and the deuterium storage layer 3 with the thickness of 3-5 mu m and the sputtering resistant layer 1 with the thickness of 200-500nm are respectively obtained.
4) Performing in-situ heat treatment in a magnetron sputtering device at 500+ -50deg.C for 500+ -20 min with vacuum degree less than 10 -4 Pa; the thickness of the formed interdiffusion solid solution transition layer is 0.3-1 mu m.
And then the neutron target is placed on a neutron source for testing, the power from the D ion beam to the neutron target is about 10-30kW, and the service life of the neutron target is improved by 300% compared with that of the neutron target prepared from the same material under the condition that the neutron yield is kept in a stable state.
Example 2
In the neutron target of this embodiment, the material of the substrate 4 is Mo alloy.
The hydrogen storage isotope layer 3 is a deuterium storage layer and is made of TiZrNbTa alloy. And smelting and forming the TiZrNbTa alloy according to the design proportion by adopting a suction casting method, rolling an ingot, and processing the ingot into the target size suitable for magnetron sputtering.
The sputtering-resistant layer 1 is Ag metal.
The specific preparation process of the neutron target is as follows:
1) And (3) carrying out rough grinding and fine grinding on the surface of the Mo alloy substrate 4 to ensure that the roughness of the surface of the substrate 4 is 0.8-1.6 mu m, and then sequentially cleaning in acetone, ethanol and deionized water for 20min each time.
2) Extruding the surface of the substrate 4 by using a prefabricated conical boss die, wherein the extruding pressure is 960MPa, and maintaining the pressure for 10min, so that the specific size of the pit is as follows: the pits have a diameter of 0.8mm and a depth of 0.4mm, and are arranged at a distance of 1.5 mm.
3) After the surface treatment of the substrate 4 is finished, a deuterium storage layer and a sputtering resistant layer 1 are plated on the surface of the substrate 4 in sequence under the protection of Ar (99.999%) by adopting a magnetron sputtering method, the plating pressure is less than 3Pa, the plating power is less than 200W, the plating time is 30-120min, and the deuterium storage layer 3 with the thickness of 3-5 mu m and the sputtering resistant layer 4 with the thickness of 300-500nm are respectively obtained.
4) Performing heat treatment in magnetron sputtering at 400+ -50deg.C for 600+ -30min with vacuum degree less than 10 -4 Pa; by diffusion at high temperatureThe thickness of the formed interdiffusion solid solution transition layer is 0.3-1 mu m.
And then the neutron target is placed on a neutron source for testing, the power from the D ion beam to the neutron target is about 10-30kW, and the service life of the neutron target is improved by 220% compared with that of the neutron target prepared from the same material under the condition that the neutron yield is kept in a stable state.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "center", "thickness", "upper", "lower", "top", "bottom", "inner", "outer", etc. are directions or positional relationships based on the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or element to be referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A neutron target based on in-situ growth, which is characterized by comprising a substrate (4), wherein one side of the substrate (4) is provided with a plurality of pits; a hydrogen storage isotope layer (3) and a sputtering resistant layer (1) are sequentially arranged on one side surface of the substrate (4);
the hydrogen storage isotope layer (3) and the sputtering-resistant layer (1) are recessed towards the substrate (4) at positions corresponding to the pits, so that the surface of the sputtering-resistant layer (1) is provided with a plurality of sputtering well pits (2).
2. The neutron target based on in-situ growth according to claim 1, wherein the sputtering well pit (2) is in an inverted conical shape, and the relation between the large end diameter D and the depth h is D/h not less than 0.38.
3. A neutron target based on in-situ growth according to claim 2, characterised in that the relation between the distance a between the centres of the large ends of adjacent sputter well pits (2) and the large end diameter D is
4. The neutron target of claim 2, wherein the diameter D of the large end is 0.2-2 mm.
5. The neutron target based on in-situ growth according to any one of claims 1 to 4, wherein the material of the sputter-resistant layer (1) comprises one or more of ceramics, tungsten alloys, palladium alloys, tantalum alloys, nickel alloys, and the thickness of the sputter-resistant layer (1) ranges from 100 to 500nm;
the material of the hydrogen storage isotope layer (3) comprises one or more of titanium, nickel, zirconium, magnesium, molybdenum, aluminum, vanadium, tantalum and rare earth elements, and the thickness of the hydrogen storage isotope layer (3) is 0.5-5 mu m;
the material of the substrate (4) is copper, copper alloy, silver alloy, molybdenum or molybdenum alloy.
6. The method for preparing an in-situ growth-based neutron target according to any one of claims 1 to 5, comprising the following steps:
s1, machining a plurality of pits on one side of the substrate (4);
s2, sequentially preparing a hydrogen storage isotope layer (3) and a sputtering-resistant layer (1) on one side of the substrate (4) in an in-situ growth mode, enabling the hydrogen storage isotope layer (3) to form the same structure as the pits, and enabling the surface of the sputtering-resistant layer (1) to form a plurality of sputtering well pits (2).
7. The method for preparing a neutron target based on in-situ growth according to claim 6, wherein before step S1 is performed, one side surface of the substrate (4) is polished to have a roughness of 0.1-3.2 μm, and then the substrate surface is sequentially cleaned with acetone, ethanol and deionized water for 15-30min each time.
8. The method of claim 6, wherein in step S1, the method of processing the plurality of pits is surface extrusion; the extrusion pressure is 5-20MPa greater than the material yield strength of the substrate (4), and the extrusion pressure is maintained for 1-10min.
9. The method for preparing a neutron target based on in-situ growth according to claim 6, wherein in the step S2, the in-situ growth mode is a magnetron sputtering method; the method comprises the following steps:
coating a film on one side of the substrate (4) by using corresponding materials in sequence in an inert gas environment by using a magnetron sputtering device, and obtaining the hydrogen storage isotope layer (3) and the sputtering resistant layer (1); wherein, the coating pressure is less than 10Pa, and the power is less than 500W.
10. The method of claim 6, further comprising the step of S3:
s3, performing in-situ heat treatment to enable the substrate (4) and the hydrogen storage isotope layer (3) to be mutually diffused at the interface between the substrate and the hydrogen storage isotope layer and form a solid solution transition layer;
the in-situ heat treatment is high-temperature diffusion treatment, and the high-temperature diffusion treatment is carried out under vacuum degree of less than 10 -4 And the high-temperature diffusion treatment is carried out under the condition of Pa, wherein the temperature of the high-temperature diffusion treatment is 500+/-50 ℃ and the time is 500+/-20 min.
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| GB1164780A (en) * | 1967-09-15 | 1969-09-24 | Commissariat Energie Atomique | Neutron-Generating Targets |
| US4055686A (en) * | 1976-02-20 | 1977-10-25 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Method of forming metal hydride films |
| GB2033651A (en) * | 1978-10-13 | 1980-05-21 | Philips Nv | Neutron generators |
| CN109699114A (en) * | 2019-02-18 | 2019-04-30 | 中国科学院合肥物质科学研究院 | A kind of MULTILAYER COMPOSITE neutron-producing target and preparation method thereof |
| CN109729637A (en) * | 2019-03-05 | 2019-05-07 | 吉林大学 | A kind of D-D neutron tube target and preparation process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100067640A1 (en) * | 2008-09-12 | 2010-03-18 | Willis Carl A | High-Power-Density Lithium Target for Neutron Production |
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| GB1164780A (en) * | 1967-09-15 | 1969-09-24 | Commissariat Energie Atomique | Neutron-Generating Targets |
| US4055686A (en) * | 1976-02-20 | 1977-10-25 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Method of forming metal hydride films |
| GB2033651A (en) * | 1978-10-13 | 1980-05-21 | Philips Nv | Neutron generators |
| CN109699114A (en) * | 2019-02-18 | 2019-04-30 | 中国科学院合肥物质科学研究院 | A kind of MULTILAYER COMPOSITE neutron-producing target and preparation method thereof |
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