CN113249694B - Sputtering inner plating black cavity and preparation method thereof - Google Patents
Sputtering inner plating black cavity and preparation method thereof Download PDFInfo
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- CN113249694B CN113249694B CN202110517710.1A CN202110517710A CN113249694B CN 113249694 B CN113249694 B CN 113249694B CN 202110517710 A CN202110517710 A CN 202110517710A CN 113249694 B CN113249694 B CN 113249694B
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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
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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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
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic 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 discloses a sputtering inner plating black cavity and a preparation method thereof, belonging to the technical field of vacuum coating and the technical field of laser inertial confinement fusion target preparation. The black cavity coating prepared by the method has controllable wall thickness uniformity and good binding force with the sleeve. Compared with the traditional black cavity, the method does not need to remove the mandrel by corrosion, thereby avoiding the influence of the corrosion process on the black cavity; the sleeve is provided with the micropore structure in advance, so that the damage of the black cavity layer processing micropore structure to the black cavity is avoided; the sputtering inner plating black cavity layer is tightly combined with the sleeve, so that the heat conduction of the black cavity of the sleeve and the regulation and control of a temperature field are facilitated; the sleeve and the black cavity are integrated, so that the mechanical property of the black cavity is improved, and the assembly difficulty is reduced; the preparation method of the sputtering inner plating black cavity has high efficiency and good process stability.
Description
Technical Field
The invention relates to the technical field of vacuum coating and the technical field of laser inertial confinement fusion target preparation, in particular to a sputtering inner plating black cavity and a preparation method thereof.
Background
In the indirect drive laser inertial confinement fusion research, laser is injected into a black cavity mainly made of a high-Z metal material, and laser energy is converted into X-ray energy through the interaction of the laser and a black cavity target wall material; then forming a high-temperature, clean and uniform thermal radiation field under the constraint of the black cavity target wall; and finally, compressing the fusion fuel to generate implosion by utilizing the interaction of the X-ray radiation and the spherical target pellets filled with the fuel, thereby realizing the controllable nuclear fusion. It can be seen that the black cavity plays a crucial role as an indirectly driven energy conversion unit.
For a long time, a black cavity mainly made of a high-Z metal material is mainly prepared by an outer plating method, which specifically comprises the following steps: firstly, turning a metal Al or Cu mandrel with a required surface structure; then preparing a black cavity coating with the required material thickness (7-50 mu m) on the outer surface of the mandrel by a sputtering and electroplating method, and finishing the processing of microstructures such as required diagnosis holes and the like; and finally, removing the mandrel material to obtain the required black cavity. The traditional preparation method of the outer black plating cavity is complex in process, extremely high in requirements on the machining precision, the coating process and the corrosion process of the outer surface of the mandrel, and particularly when the black cavity material contains metal U, the mandrel corrosion is extremely difficult to limit by the chemical activity of the metal U. Even if the corrosion is successful, the formed thin-wall cavity is easy to deform, delaminate, crack and the like in the processing and assembling processes, and the process is difficult to control and poor in stability. In addition, when a target pellet fuel ice layer is prepared in the black cavity, the black cavity and the heat conducting sleeve cannot form surface contact, and the temperature field in the black cavity is difficult to regulate and control due to heat-resistant media such as gaps.
Disclosure of Invention
In order to overcome the defects of the existing outer black plating cavity, the invention aims to solve the technical problems that: provides a sputtering inner plating black cavity and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the utility model provides a black chamber of plating in sputtering, includes the sleeve and sets up the cladding material on the sleeve inner wall, the cladding material adopts the sputtering mode to deposit metal on the sleeve inner wall.
Further, the inner cavity of the sleeve is a cavity-shaped structure formed by a cylinder, a multi-section cylinder, a spherical cylinder, an ellipsoid cylinder or a combination of the above shapes.
Further, the inner wall of the sleeve is provided with a micropore structure.
Further, the sleeve is made of Cu, Al or an alloy material of the Cu and the Al, and the plating layer is made of Au, U, AuB, UN or a combination layer or a mixed layer of the Au, the U, the AuB and the UN.
A preparation method of a sputtering inner plating black cavity comprises the following steps:
A. sequentially putting the sleeve into acetone, ethanol and deionized water for ultrasonic cleaning, and then blowing the sleeve dry by high-purity nitrogen;
B. masking the part of the sleeve not needing the coating, then placing the sleeve on a sample table, and enabling the distance from the center of the sample table to the center of the sputtering target to be 80-150 mm, wherein the normal line of the rotation center of the sample table and the central axis of the sputtering target form an included angle of 30-45 degrees;
C. vacuumizing the sputtering vacuum chamber, and then introducing argon;
D. etching the inner wall of the sleeve on the sample table by utilizing an ion beam;
E. sputtering on the inner wall of the sleeve by using a sputtering target to form a pre-coating layer with the thickness of 50-300 nm, and then stopping sputtering;
F. carrying out heat treatment on the sleeve at 150-300 ℃, wherein the heat treatment time is 30-300 min;
G. when the sleeve is cooled to 20-30 ℃, continuing sputtering until the coating reaches the required thickness, and then stopping coating;
H. and (4) turning the sleeve up and down, keeping the position unchanged, continuing sputtering to the required thickness, and stopping coating to finish the preparation of the whole inner black-plated cavity.
Further, in step C, the degree of vacuum of the sputtering vacuum chamber is first brought to 1X 10-7Pa～1×10-5Pa, then introducing argon gas, and maintaining the vacuum degree of the sputtering vacuum chamber at 0.1 Pa-0.6 Pa.
And further, in the step E, before sputtering, a baffle is arranged between the sputtering target and the sleeve, then pre-sputtering is carried out for 5-10 min, and finally the baffle is taken down, and sputtering is carried out on the inner wall of the sleeve.
And further, an intermittent coating mode is adopted in the sputtering process in the step G, the sputtering is stopped for 5-20 min after 20min of each period, and the coating is stopped until the required thickness is reached.
And further, in the step G, a double-target co-sputtering mode is adopted for coating, and the Au target and the B target are symmetrically arranged along the normal of the rotation center of the sample table, wherein the Au target is direct current sputtering, and the B target is radio frequency sputtering.
Further, the B target radio frequency sputtering is replaced by AuB direct current sputtering.
The invention has the beneficial effects that:
1. compared with a black cavity plated outside the mandrel, the sputtering inner black cavity does not need to be corroded to remove the mandrel, so that the preparation difficulty of the black cavity is effectively reduced;
2. the sputtering inner plating black cavity does not need to directly process a microstructure on the black cavity layer, but a related microstructure is pre-arranged on the sleeve, and the direct forming is carried out without secondary processing after the plating of the black cavity layer is finished, so that the problem of black cavity layer damage caused by secondary processing is avoided;
3. the wall thickness of a sleeve used for sputtering the inner plating black cavity can be more than 100 mu m, the mechanical property is stable, the sleeve is not easy to deform in the assembling process, and the assembling difficulty is reduced;
4. the sputtering inner plating black cavity is in seamless surface contact with the sleeve, the temperature field is regulated and controlled simply and stably, and the preparation of the target pellet ice layer in the sputtering inner plating black cavity is facilitated;
5. the sputtering inner plating black cavity can realize the small-batch preparation of 1-30 black cavities, and has simple and convenient operation, low cost and high efficiency.
Drawings
FIG. 1 is a CT test chart of an inner plating black cavity.
FIG. 2 is a scanning electron micrograph of the cross section of the inner plating black cavity layer at different positions.
Labeled as 1-sleeve, 2-plating.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
The traditional black cavity is generally prepared by an external plating mode, the mandrel material in the black cavity needs to be removed by corrosion after the black cavity is plated, the problems of deformation, falling, cracking and the like of a black cavity layer are easily caused by corrosion, particularly, a U-shaped black cavity is contained, a protective layer needs to be additionally plated before the mandrel is removed, and the preparation process is very harsh. The conventional black cavity layer needs to be secondarily processed with microstructures such as star mango holes and the like after being plated, the processing process has high requirements on the stability of the black cavity layer and the binding force between the black cavity layer and a mandrel, and particularly the processing cost of a U-shaped black cavity is extremely high. And after preparation, the black cavity is required to be arranged in the sleeve in an equipment mode, the thickness of the black cavity is generally 7-50 mu m, and the black cavity is easy to deform in different degrees under the action of external force, so that the assembly difficulty is high. After the black chamber and the sleeve are assembled, the black chamber is in local contact with the sleeve, a gap exists, the sleeve is different from the real temperature in the black chamber when being cooled, and the temperature field regulation in the black chamber and the uniform preparation of the target pellet fuel ice layer in the black chamber are not facilitated.
The sputtering inner plating black cavity provided by the invention comprises a sleeve 1 and a plating layer 2 arranged on the inner wall of the sleeve 1, wherein the plating layer 2 is used for depositing metal powder on the inner wall of the sleeve 1 in a sputtering mode, as shown in figure 1. The sputtering inner plating black cavity does not need to be corroded to remove the mandrel, and the preparation difficulty of the black cavity is effectively reduced. And the sputtering inner plating black cavity does not need to directly process a microstructure on the black cavity layer, but the related microstructure is pre-arranged on the sleeve, and the direct forming is not needed after the plating of the black cavity layer is finished, so that the problem of damage of the black cavity layer caused by secondary processing is avoided. The wall thickness of the sleeve used for sputtering the inner black plating cavity can be larger than 100 mu m, the mechanical property is stable, the sleeve is not easy to deform in the assembling process, and the assembling difficulty is reduced. In addition, the sputtering inner plating black cavity is in seamless surface contact with the sleeve, and the temperature field is simply and stably regulated and controlled, so that the preparation of the target pellet ice layer in the sputtering inner plating black cavity is facilitated. And the sputtering inner plating black cavity can realize the small-batch preparation of 1-30 black cavities, and has simple and convenient operation, low cost and high efficiency.
The sleeve 1 can adopt different shapes according to different use requirements, and the inner cavity of the sleeve can be a cylindrical shape, a multi-section cylindrical shape, a spherical cylinder shape, an ellipsoidal cylinder shape or a cavity-shaped structure formed by combining the shapes. In order to directly form microstructures such as star-shaped mango holes and the like on the black cavity coating, a microporous structure can be arranged on the inner wall of the sleeve 1 in advance, and the needed microstructures can be formed at the microporous structure after sputtering inner plating is finished.
The material is similar to that of a common outer black plating cavity, the material of the sleeve 1 can be Cu, Al or an alloy material of Cu and Al according to different use requirements, and the material of the plating layer 2 can be Au, U, AuB, UN or a combination layer or a mixed layer of the Au, the U, the AuB and the UN.
The preparation method of the sputtering inner plating black cavity comprises the following steps:
A. sequentially putting the sleeve into acetone, ethanol and deionized water for ultrasonic cleaning, and then blowing the sleeve dry by high-purity nitrogen;
B. masking the part of the sleeve not needing the coating, then placing the sleeve on a sample table, and enabling the distance from the center of the sample table to the center of the sputtering target to be 80-150 mm, wherein the normal line of the rotation center of the sample table and the central axis of the sputtering target form an included angle of 30-45 degrees;
C. vacuumizing the sputtering vacuum chamber, and then introducing argon;
D. etching the inner wall of the sleeve on the sample table by utilizing an ion beam;
E. sputtering on the inner wall of the sleeve by using a sputtering target to form a pre-coating layer with the thickness of 50-300 nm, and then stopping sputtering;
F. carrying out heat treatment on the sleeve at 150-300 ℃, wherein the heat treatment time is 30-300 min;
G. when the sleeve is cooled to 20-30 ℃, continuing sputtering until the coating reaches the required thickness, and then stopping coating;
H. and (4) turning the sleeve up and down, keeping the position unchanged, continuing sputtering to the required thickness, and stopping coating to finish the preparation of the whole inner black-plated cavity.
The step A aims to remove pollutants such as grease and the like left on the sleeve in the machining stage through cleaning, so that the bonding force between a subsequent coating and the sleeve is prevented from being influenced. The high-purity nitrogen refers to nitrogen with the nitrogen content of more than 99.99%, and the liquid left on the sleeve is directly and quickly blown away by utilizing the high-speed nitrogen instead of being slowly evaporated, so that impurities left on the sleeve can be prevented from being attached to the sleeve.
And B, masking the sleeve in order to control the sputtering part and prevent the target from sputtering the surfaces of the tool clamp and the rest parts of the sleeve. The distance from the center of the sample table to the center of the sputtering target is controlled to be 80-150 mm, and the speed of sputtering metal is fastest in the range, so that the control of the thickness and the deposition rate of a coating is facilitated. Because the cavity of the sleeve is generally small in size, and the inner diameter and the height of the cavity are only 2-3 mm, the normal line of the rotating center of the sample platform and the central axis of the sputtering target form an included angle of 30-45 degrees, and metal can be better deposited on the inner wall of the sleeve. Also because the cavity in the sleeve is less, the uniformity of the thickness of the coating can not be ensured only by sputtering from one end, so that a step H is needed, the sleeve is turned over up and down and then sputtered from the other end, and the uniformity of the whole coating is ensured.
In step C, the vacuum degree of the sputtering vacuum chamber is firstly made to reach 1 x 10-7Pa～1×10-5Pa, then introducing argon gas, and maintaining the vacuum degree of the sputtering vacuum chamber at 0.1 Pa-0.6 Pa. The reasonable air pressure protection can ensure the stable and reliable work of the sputtering target and ensure that the plating layer is not interfered by the outside air.
And D, etching the inner wall of the sleeve to remove impurities such as an oxide layer and the like left on the inner wall of the sleeve in the machining process on one hand, and to enable the inner wall of the sleeve to reach certain nano-grade roughness on the other hand, so that the binding force with the coating is improved.
And E, before sputtering, arranging a baffle between the sputtering target and the sleeve, then carrying out pre-sputtering for 5-10 min, and finally taking down the baffle to sputter the inner wall of the sleeve. The purpose of pre-sputtering is to eliminate air or impurities in the sputtering target, so that the sputtering target reaches the optimal working state, and the stability of the subsequent sleeve sputtering is ensured.
When the sleeve is sputtered, the method adopts two stages, wherein the first stage is to form a pre-plating layer with the thickness of 50-300 nm, then the pre-plating layer is subjected to heating treatment, and the metal in the plating layer can be diffused among sleeve base materials through heat treatment, so that the binding force between the plating layer and the sleeve is improved; and normal sputtering is carried out again in the second stage until the required thickness is reached.
And G, sputtering for 20min in each period, stopping for 5-20 min, and stopping coating until the required thickness is reached. After a period of sputtering, a certain period of time is reserved for thermal stress relaxation and the like of the sputtered coating, and then sputtering is carried out, so that the compactness and the structural strength of the coating can be improved by repeating the steps.
For some black cavities requiring alloy as a coating, such as alloy of Au and B, a double-target co-sputtering mode can be adopted for coating in the step G, the Au targets and the B targets are symmetrically arranged along the normal of the rotation center of the sample stage, and according to different materials, the Au targets are preferably subjected to direct current sputtering, and the B targets are preferably subjected to radio frequency sputtering. Wherein, the B target radio frequency sputtering can be replaced by AuB direct current sputtering.
The invention is further illustrated by the following specific examples.
The first embodiment is as follows:
by adopting the preparation method of the sputtering inner plating black cavity, the inner plating black cavity is carried out on the sleeve with the inner diameter of 2.6mm and the inner height of 2.3mm, the black cavity is made of Au and B alloy, and the specific preparation process is as follows:
step one, putting the sleeve into sufficient acetone, ethanol and deionized water, sequentially carrying out ultrasonic cleaning for 10min, and drying by using high-purity nitrogen;
secondly, placing a sleeve mask in a circular area with the central diameter of 50mm of the sample stage, wherein the axis of the sleeve is vertical to the plane of the sample stage; the distance from the center of the sample table to the center of the sputtering target is 100mm, and the normal line of the rotating center of the sample table forms an angle of 35 degrees with the central axis of the sputtering target.
Step three, pumping by a mechanical pump and a molecular pumpThe vacuum degree of the sputtering vacuum chamber reaches 1 x 10-5Pa, then filling high-purity argon, and adjusting a gate valve to maintain the vacuum degree of the sputtering vacuum chamber at 0.3 Pa;
and step four, etching the inner wall of the sleeve on the sample table for 15min by using ion beams, wherein the rotating speed of the sample table is 10 rpm.
Fifthly, arranging a baffle between the sputtering target Au and the sputtering target B and the sleeve, and closing the baffle to pre-sputter for 5min under the power of 100W;
step six, opening a baffle between the sputtering target Au and the sleeve, sputtering for 15min on the inner wall of the sleeve, and stopping sputtering after a pre-plating layer with the thickness of 120nm is formed;
step seven, carrying out heat treatment for 100 mins at 200-300 ℃ by using a sample stage in-situ heating device;
step eight, when the sleeve is cooled to 25 ℃, simultaneously opening an Au target and a B target for co-sputtering, performing direct current sputtering on the Au target, performing radio frequency sputtering on the B target at the power of 20W, and performing 180W; intermittent coating is adopted in the sputtering process, and the sputtering is stopped for 10min at each period of 20min until the required thickness is reached, and the coating is stopped;
and step nine, keeping the upper and lower overturning positions of the sleeve unchanged, continuously adopting intermittent coating sputtering to reach the required thickness, and then stopping coating.
After the plating is finished, scanning different positions of the black cavity section by adopting an electron microscope to obtain a photo shown in figure 2, and analyzing the thickness of the black cavity section to obtain data shown in the following table:
table I, black cavity section thickness distribution test results
| Position of | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Thickness (um) | 10.57 | 10.62 | 10.82 | 10.64 | 10.45 | 10.61 | 10.13 |
Therefore, the black cavity with uniform thickness can be prepared by adopting the method for sputtering the inner plating black cavity, and the bonding force between the black cavity and the sleeve is good. Compared with the traditional black cavity: the method does not need to remove the mandrel by corrosion, thereby avoiding the influence of the corrosion process on the black cavity; the sleeve is provided with the micropore structure in advance, so that the damage of the black cavity layer processing micropore structure to the black cavity is avoided; the sputtering inner plating black cavity layer is tightly combined with the sleeve, so that the heat conduction of the black cavity of the sleeve and the regulation and control of a temperature field are facilitated; the sleeve and the black cavity are integrated, so that the mechanical property of the black cavity is improved, and the assembly difficulty is reduced; the preparation method of the sputtering inner plating black cavity has high efficiency, good process stability and good application prospect.
Claims (9)
1. The utility model provides a black chamber of plating in sputtering, includes sleeve (1) and cladding material (2) of setting on sleeve (1) inner wall, characterized by: the plating layer (2) adopts a sputtering mode to deposit metal on the inner wall of the sleeve (1), and the inner wall of the sleeve (1) is provided with a microporous structure.
2. The sputtering inner black plating chamber as claimed in claim 1, wherein: the inner cavity of the sleeve (1) is a cavity-shaped structure formed by a cylinder, a multi-section cylinder, a spherical cylinder, an ellipsoid cylinder or a combination of the above shapes.
3. The sputtering inner black plating chamber as claimed in claim 1, wherein: the sleeve (1) is made of Cu, Al or an alloy material of the Cu and the Al, and the plating layer (2) is made of Au, U, AuB, UN or a combined layer or a mixed layer of the Au, the U, the AuB and the UN.
4. A preparation method of a sputtering inner plating black cavity is characterized by comprising the following steps:
A. sequentially putting the sleeve into acetone, ethanol and deionized water for ultrasonic cleaning, and then blowing the sleeve dry by high-purity nitrogen;
B. masking the part of the sleeve not needing the coating, then placing the sleeve on a sample table, and enabling the distance from the center of the sample table to the center of the sputtering target to be 80-150 mm, wherein the normal line of the rotation center of the sample table and the central axis of the sputtering target form an included angle of 30-45 degrees;
C. vacuumizing the sputtering vacuum chamber, and then introducing argon;
D. etching the inner wall of the sleeve on the sample table by utilizing an ion beam;
E. sputtering on the inner wall of the sleeve by using a sputtering target to form a pre-coating layer with the thickness of 50-300 nm, and then stopping sputtering;
F. carrying out heat treatment on the sleeve at 150-300 ℃, wherein the heat treatment time is 30-300 min;
G. when the sleeve is cooled to 20-30 ℃, continuing sputtering until the coating reaches the required thickness, and then stopping coating;
H. and (4) turning the sleeve up and down, keeping the position unchanged, continuing sputtering to the required thickness, and stopping coating to finish the preparation of the whole inner black-plated cavity.
5. The method for preparing the sputtering inner plating black cavity as claimed in claim 4, wherein the method comprises the following steps: in step C, the vacuum of the sputtering vacuum chamber is firstly madeThe degree reaches 1 x 10-7Pa～1×10-5Pa, then introducing argon gas, and maintaining the vacuum degree of the sputtering vacuum chamber at 0.1 Pa-0.6 Pa.
6. The method for preparing the sputtering inner plating black cavity as claimed in claim 4, wherein the method comprises the following steps: and E, before sputtering, arranging a baffle between the sputtering target and the sleeve, then carrying out pre-sputtering for 5-10 min, and finally taking down the baffle to sputter the inner wall of the sleeve.
7. The method for preparing the sputtering inner plating black cavity as claimed in claim 4, wherein the method comprises the following steps: and G, sputtering in an intermittent coating mode, stopping for 5-20 min after 20min of sputtering in each period, and stopping coating until the required thickness is reached.
8. The method for preparing a sputtering inner plating black cavity as claimed in claim 7, wherein the method comprises the following steps: and G, coating by adopting a double-target co-sputtering mode, wherein the Au target and the B target are symmetrically arranged along the normal of the rotation center of the sample table, the Au target is DC sputtering, and the B target is radio frequency sputtering.
9. The method for preparing a sputtering inner plating black cavity as claimed in claim 8, wherein: the B target radio frequency sputtering is replaced by AuB direct current sputtering.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB755526A (en) * | 1953-10-12 | 1956-08-22 | Metallurg Company Ltd Soc Gen | Improvements relating to multi-cavity magnetrons |
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