CN115354285A - 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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- CN115354285A CN115354285A CN202210897639.9A CN202210897639A CN115354285A CN 115354285 A CN115354285 A CN 115354285A CN 202210897639 A CN202210897639 A CN 202210897639A CN 115354285 A CN115354285 A CN 115354285A
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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
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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
- 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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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 the surface of one side of the substrate; the hydrogen storage isotope layer and the sputtering resistant layer are recessed toward the substrate at the position of the recess, so that the surface of the sputtering resistant layer has a plurality of sputtering well recesses. Firstly, processing a plurality of pits on one side of a substrate; and then 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 the same as that of the pits, and a plurality of sputtering trap pits are formed on the surface of the sputtering resistant layer. Atoms sputtered and flying out of the surface of the neutron target can be blocked by the inner wall of the sputtering well pit and are 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 the fields of neutron photography, oil field well logging, cancer treatment, neutron security inspection, activation analysis, irradiation breeding, irradiation damage research, nuclear measurement and the like. The major neutron sources currently available are nuclear reactors, radioactive sources and accelerator-type neutron sources. The accelerator type deuterium-tritium neutron source bombards a neutron target through accelerating deuterium ion beams to generate 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 the deuterium fusion neutron generator, a neutron target is a core component that directly generates neutrons. Wherein the lifetime of the neutron target is critical to the neutron generator operating and usage costs. Currently, the commonly used neutron targets are mainly divided into prefabricated targets and self-made targets. The pre-fabricated target is generally that a single titanium film is plated on a substrate, then deuterium/tritium is absorbed by the titanium film to obtain a deuterium/tritium titanium target, the deuterium/tritium titanium target is placed in an accelerator, and the deuterium/tritium titanium target is bombarded by accelerated deuterium ion beams to generate fusion reaction to generate neutrons; the self-forming target is generally formed by plating a single titanium film on a substrate to form a titanium target, the titanium target is directly arranged in an accelerator, the accelerated deuterium ion beam bombards the titanium target and deposits 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 high-speed deuterium ion beam bombards the neutron target in the operation process, and the titanium film is subjected to the 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 the deuterium ion are transferred to the atoms on the surface of the neutron target, so that the surface atoms are splashed and lost due to the breakage 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, so that 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 the key technologies for prolonging the service life of the neutron target.
The sputtering effect is closely related to the material type. The existing 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 high-energy deuterium ion beams cannot penetrate through the sputtering-resistant film to reach the hydrogen storage isotope layer (titanium film layer) and then cannot generate fusion reaction to generate neutrons, or the number of deuterium atoms reaching the hydrogen storage isotope layer and deuterium/tritium atoms therein 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 on the order of nanometers. Since the sputtering resistant film is too thin, it is sputtered off quickly, leaving a hydrogen storage isotope layer (titanium film layer) exposed, although the sputtering rate is low. Therefore, the sputtering-resistant film prepared by the traditional method has extremely limited effect on prolonging the service life of the neutron target, and cannot meet the use requirement of the long-service-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 the surface of one side of the substrate; the hydrogen storage isotope layer and the sputtering resistant layer are sunken 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 trap pits.
On the basis of the technical scheme, the invention can be further improved as follows.
Furthermore, the pit of the sputtering trap is in an inverted cone shape, and the relation between the diameter D of the large end of the pit and the depth h is that D/h is more than or equal to 0.38.
Further, the relation between the distance a between the centers of the large ends of the adjacent sputtering trap pits and the diameter D of the large end is
Further, the diameter D of the large end is 0.2 to 2mm.
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 of the sputtering resistant layer ranges from 100 nm to 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 preparation method of the neutron target based on in-situ growth, which comprises the following steps:
s1, processing a plurality of pits on one side of the substrate;
s2, sequentially preparing a hydrogen storage isotope layer and a sputtering-resistant layer on one side of the substrate in an in-situ growth mode, enabling the hydrogen storage isotope layer to form a structure identical to that of the pit, and enabling the surface of the sputtering-resistant layer to form a plurality of sputtering trap pits.
Further, before the step S1, polishing the surface of one side of the substrate to the roughness of 0.1-3.2 μm, and then sequentially cleaning the surface of the substrate by using acetone, ethanol and deionized water, wherein the cleaning time is 15-30min each time.
Further, in the step S1, the manner of processing the plurality of pits is surface extrusion molding; the extrusion pressure is 5-20MPa higher than the material yield strength of the substrate, and the pressure is kept for 1-10min during extrusion.
Further, in the step S2, the in-situ growth mode is a magnetron sputtering method; the method comprises the following steps:
sequentially coating one side of the substrate with corresponding materials by adopting magnetron sputtering equipment in an inert gas environment to obtain 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 step S3:
s3, carrying out in-situ heat treatment to enable the substrate and the hydrogen storage isotope layer to mutually diffuse at an 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 which is small in vacuum degreeAt 10 -4 Pa, 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 well pits are formed in the surface of the sputtering-resistant layer, so that atoms sputtered and flying out of the surface of the neutron target can be blocked by the inner walls of the sputtering well pits and are redeposited in the sputtering well pits, and can not 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 well pit is obtained by in-situ growth on the pit of the substrate, instead of simply arranging the pit on the surface of the sputtering-resistant layer, so that the sputtering-resistant layer keeps 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 occluded through the pit structure, and compared with the plane connection among all layers of a common neutron target, the neutron target has stronger interface binding force, and the falling and separation conditions under the action of strong stress are effectively prevented;
(4) Compared with the common neutron target, the in-situ growth-based neutron target has the advantages that the service life of the neutron target can be prolonged by 200-300%;
(5) According to the neutron target preparation method based on in-situ growth, the in-situ growth mode is adopted, the pits are processed on the substrate, 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 bonding strength of the film interface when the sputtering trap pits are 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 as well as the hydrogen storage isotope layer and the sputtering resistant layer are diffused mutually, a solid solution transition layer is formed, and the layers are meshed mutually through the pit structure, and meanwhile, the interface bonding force between the layers is further improved;
(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 present invention;
FIG. 2 is a front view of a sputter resistant layer and sputter well pits of an in-situ grown neutron target based on the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
1. a sputter-resistant layer; 2. sputtering a well pit; 3. a hydrogen storage isotope layer; 4. a substrate.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth to illustrate, but are not to be construed to limit 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, the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 are sunken towards the substrate 4 at positions corresponding to a plurality of pits, so that the surface of the sputtering resistant layer 1 is provided with a plurality of sputtering well 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 well pits 2, through the sputtering well effect, when the neutron target is used and a high-speed deuterium ion beam bombards the surface of the neutron target, atoms on the surface of the neutron target are sputtered, the sputtered atoms are blocked by the inner walls of the sputtering well pits 2 and are redeposited in the sputtering well 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 problem of the neutron target is effectively relieved, the sputtering rate of the neutron target is reduced from the source, and the service life of the neutron target is greatly prolonged.
In addition, if the sputtering resistant layer 1 is thinned, the sputtering resistant layer can be sputtered quickly, and the hydrogen storage isotope layer 3 at the lower layer is exposed, so that the service life of the neutron target is greatly limited. The sputtering trap 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 keeps uniform thickness, and the service life of the neutron target can be ensured.
Meanwhile, the substrate 4, the hydrogen storage isotope layer 3 and the sputtering-resistant layer 1 of the neutron target are mutually occluded through the pit structure, and compared with the plane connection among all layers of a common neutron target, the neutron target has stronger interface binding force, and effectively prevents the falling and separation conditions under the action of strong stress.
The hydrogen storage isotope layer 3 may be a deuterium storage layer, a tritium storage layer, or a mixture layer of deuterium and tritium.
Preferably, the plurality of sputter well pits 2 of the present invention are uniformly arranged in a matrix.
Preferably, the pit 2 of the sputtering trap is in an inverted conical shape, and the relation between the diameter D of the large end of the pit and the depth h is that D/h is more than or equal to 0.38; by adopting the conical sputtering trap pit 2, atoms sputtered in the sputtering trap pit 2 can be blocked by the sputtering trap pit 2 to the maximum extent, and if the bottom of the sputtering trap pit 2 is set to be a flat structure, the atoms at the position can easily escape.
Preferably, the relationship between the distance a between the centers of the large ends of adjacent sputter well pits 2 and the diameter D of the large end is
If the arrangement of the sputtering well pits 2 is too dense, the material in the non-sputtering well pit 2 area can be sputtered away, and the service life of the neutron target is affected; and if the sputtering trap pits 2 are arranged too sparsely, the effect of the sputtering trap is affected, the overall sputtering resistance is reduced, and the requirements cannot be met.
Preferably, the large end diameter D 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 is in the range of 100-500nm.
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, a copper alloy, silver, a silver alloy, molybdenum or a molybdenum alloy.
According to the neutron target preparation method based on in-situ growth, a plurality of pits are processed on one side of a substrate 4, a hydrogen storage isotope layer 3 and a sputtering resistant layer 1 are sequentially prepared on one side of the substrate 4 in an in-situ growth mode, the hydrogen storage isotope layer 3 is made to form a structure the same as that of 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 interface of each layer of the substrate 4, the hydrogen storage isotope layer 3 and the sputtering-resistant layer 1 can be damaged, and even the hydrogen storage isotope layer 3 and the sputtering-resistant layer 1 are cracked and fall off, so that the preparation fails.
According to the preparation method, the pit is firstly processed on the substrate 4 by adopting an in-situ growth mode, and 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 the sputtering resistant layer 1 with the sputtering well pit 2 structure is finally prepared, thereby effectively avoiding the influence on the bonding strength of the film interface when the sputtering well pit 2 is prepared later, and improving the comprehensive mechanical property of the neutron target.
Preferably, the substrate 4 is processed by surface etching, 3D printing or surface extrusion.
Preferably, the in-situ growth mode is magnetron sputtering, thermal vacuum evaporation, pulsed laser or chemical vapor deposition.
Preferably, the preparation method of the invention comprises the following steps:
1) Polishing the surface of the substrate 4 until the roughness is 0.1-3.2 μm, and then sequentially cleaning the surface of the substrate by using acetone, ethanol and deionized water, wherein the cleaning time is 15-30min each time.
2) Extruding the surface of one side 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 kept 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 adopting magnetron sputtering equipment; the preparation is carried out in an inert gas environment every time, the film plating pressure of the magnetron sputtering equipment is less than 10Pa, and the power is less than 500W.
4) And carrying out in-situ heat treatment in magnetron sputtering equipment, and carrying out high-temperature diffusion treatment to enable the substrate 4 and the hydrogen storage isotope layer 3 to mutually diffuse at the interface between the substrate and the hydrogen storage isotope layer and form a solid solution transition layer.
Wherein the high temperature diffusion treatment temperature is 500 + -50 deg.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 μm. And obtaining the neutron target after the in-situ heat treatment is finished.
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 as well as the hydrogen storage isotope layer 3 and the sputtering resistant layer 1 are mutually diffused and form a solid solution transition layer, and the layers are mutually occluded through a pit structure, and simultaneously, the interface bonding force between the layers is further improved.
Since the sputtering-resistant layer 1 is thin, a transition layer formed with the hydrogen storage isotope layer 3 can be theoretically formed, but the transition layer is thin and can be ignored.
The technical solution of the present invention is illustrated by the following 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 made of Ti55Mo45 alloy, the Ti55Mo45 alloy is smelted and formed according to the designed proportion by a vacuum smelting method, and cast ingots are rolled and processed into target materials with the size suitable for magnetron sputtering.
The material of the sputter-resistant layer 1 is pure Pd.
The neutron target of this embodiment is prepared by sequentially plating a deuterium storage layer 3 and a sputtering-resistant layer 1 on the surface of a substrate 4, and specifically prepared by the following steps:
1) And performing coarse grinding and fine grinding on the surface of the CrZrCu substrate 4 to enable the roughness of the surface of the substrate 4 to be less than 3.2 microns, and then sequentially cleaning the surface with acetone, ethanol and deionized water for 15-30min each time.
2) And extruding the surface of the substrate 4 by using a pre-processed conical boss die, wherein the extrusion pressure is 340MPa, and the pressure is maintained for 5min. The specific dimensions of the pits were obtained 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 of the substrate 4 is treated, the deuterium storage layer and the sputtering resistant layer 1 are sequentially plated on the surface of the substrate 4 by adopting a magnetron sputtering method under the protection of Ar (99.999%), the plating pressure is less than 1Pa, the plating power is less than 200W, and the plating time is 30-240min, so that 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) Carrying out in-situ heat treatment in a magnetron sputtering device at the temperature of 500 +/-50 ℃ for 500 +/-20 min and the vacuum degree of less than 10 -4 Pa; the thickness of the formed interdiffusion solid solution transition layer is 0.3-1 μm.
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 the neutron target prepared by the same material under the condition that the neutron yield is kept in a stable state.
Example 2
In the neutron target of the present 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. Smelting and forming TiZrNbTa alloy according to a designed proportion by adopting a suction casting method, rolling cast ingots, and processing into a target material 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 performing coarse grinding and fine grinding on the surface of the substrate 4 of the Mo alloy to ensure that the roughness of the surface of the substrate 4 is 0.8-1.6 mu m, and then sequentially cleaning the substrate 4 with acetone, ethanol and deionized water for 20min each time.
2) And extruding the surface of the substrate 4 by using a pre-processed conical boss die, wherein the extrusion pressure is 960MPa, and the pressure is maintained for 10min, so that the concrete 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 of the substrate 4 is treated, the surface of the substrate 4 is sequentially plated with a deuterium storage layer and a sputtering resistant layer 1 by a magnetron sputtering method under the protection of Ar (99.999%), the plating pressure is less than 3Pa, the plating power is less than 200W, and the plating time is 30-120min, so that 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) Heat treatment is carried out in the magnetron sputtering at 400 +/-50 ℃ for 600 +/-30 min, and the vacuum degree is less than 10 -4 Pa; through high-temperature diffusion treatment, the thickness of the formed interdiffusion solid solution transition layer is 0.3-1 μm.
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 the neutron target prepared by 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 terms "center", "thickness", "upper", "lower", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "above," and "over" a second feature may be directly on or obliquely above the second feature, or simply mean that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like 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 invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer 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, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (10)
1. The neutron target based on in-situ growth 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 the surface of one side of the substrate (4);
the hydrogen storage isotope layer (3) and the sputtering resistant layer (1) are recessed toward the substrate (4) at positions corresponding to the plurality of pits, so that the surface of the sputtering resistant layer (1) has a plurality of sputtering well pits (2).
2. The in-situ growth based neutron target according to claim 1, wherein the sputtering trap pit (2) is an inverted cone with a large end diameter D in relation to a depth h, wherein D/h is greater than or equal to 0.38.
3. Root of herbaceous plantsThe in-situ growth based neutron target according to claim 2, wherein the relationship between the distance a between the centers of the large ends of the adjacent sputtering trap pits (2) and the diameter D of the large end is
4. The in-situ growth based neutron target of claim 2, wherein the diameter D of the large end has a value of 0.2 mm to 2mm.
5. The in-situ growth based neutron target according to any one of claims 1 to 4, wherein the material of the sputtering resistant layer (1) comprises one or more of ceramic, tungsten alloy, palladium alloy, tantalum alloy and nickel alloy, and the thickness of the sputtering resistant layer (1) is in the range of 100-500nm;
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 substrate (4) is made of copper, copper alloy, silver alloy, molybdenum or molybdenum alloy.
6. The method for preparing the neutron target based on in-situ growth according to any one of claims 1 to 5, characterized by comprising the following steps:
s1, processing 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 a structure the same as that of the pits, and enabling the surface of the sputtering resistant layer (1) to form a plurality of sputtering trap pits (2).
7. The in-situ growth-based neutron target preparation method according to claim 6, wherein before the step S1, one side surface of the substrate (4) is polished to a roughness of 0.1-3.2 μm, and then the substrate surface is sequentially cleaned by acetone, ethanol and deionized water, wherein the cleaning time is 15-30min each time.
8. The in-situ growth based neutron target preparation method according to claim 6, wherein in the step S1, the manner of processing the plurality of pits is surface extrusion molding; the extrusion pressure is 5-20MPa higher than the material yield strength of the substrate (4), and the pressure is kept for 1-10min during extrusion.
9. The in-situ growth-based neutron target preparation method 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:
sequentially coating one side of the substrate (4) with corresponding materials by adopting magnetron sputtering equipment in an inert gas environment to obtain 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 in-situ growth-based neutron target preparation method according to claim 6, wherein after the step S2 is finished, the method further comprises the step S3:
s3, carrying out in-situ heat treatment to enable the substrate (4) and the hydrogen storage isotope layer (3) to mutually diffuse 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 the condition that the vacuum degree is less than 10 -4 Pa, and the high-temperature diffusion treatment is carried out at the temperature of 500 +/-50 ℃ for 500 +/-20 min.
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