CN114574829B - Micro deep hole inner coating process and coating device - Google Patents
Micro deep hole inner coating process and coating device Download PDFInfo
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- CN114574829B CN114574829B CN202210219391.0A CN202210219391A CN114574829B CN 114574829 B CN114574829 B CN 114574829B CN 202210219391 A CN202210219391 A CN 202210219391A CN 114574829 B CN114574829 B CN 114574829B
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- 238000000576 coating method Methods 0.000 title claims abstract description 57
- 239000011248 coating agent Substances 0.000 title claims abstract description 42
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 230000008878 coupling Effects 0.000 claims abstract description 12
- 238000010168 coupling process Methods 0.000 claims abstract description 12
- 238000005859 coupling reaction Methods 0.000 claims abstract description 12
- 238000005516 engineering process Methods 0.000 claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 12
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 238000004544 sputter deposition Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 23
- 230000008569 process Effects 0.000 claims description 17
- 229910052786 argon Inorganic materials 0.000 claims description 14
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- -1 argon ions Chemical class 0.000 claims description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000007872 degassing Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000001764 infiltration Methods 0.000 abstract description 5
- 230000008595 infiltration Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 4
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- 239000010408 film Substances 0.000 description 37
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Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- C23C14/3485—Sputtering using pulsed power to the target
-
- 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
- C23C14/50—Substrate holders
- C23C14/505—Substrate holders for rotation of the substrates
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application provides a micro deep hole inner coating process and a coating device, which relate to the technical field of material science and engineering and are used for coating a workpiece with a hole. The micro deep hole inner coating process comprises the following steps: placing the workpiece and the magnetic control target oppositely to enable the workpiece to be in a autorotation state; carrying out gas ion cleaning on the workpiece; and (3) coating the workpiece, and performing sputter coating on the workpiece by adopting a high-power pulse magnetron sputtering technology, and completing the deposition of the film layers on the surface of the workpiece and the surface of the side wall of the hole by matching with the high-power pulse bias coupled on the workpiece. The micro deep hole inner coating process of the application utilizes the characteristics of high plasma density and high plasma ionization rate of the high-power pulse magnetron sputtering technology to place the workpiece in front of the magnetron target for autorotation, and then utilizes the coupling bias to attract ions into the hole, so that the hole is in a plasma infiltration state, and the plasma is deposited on the side wall of the hole, thereby not only effectively improving the uniformity of the coating film layer on the side wall of the micropore, but also improving the adhesive force of the film layer and the quality of the film layer.
Description
Technical Field
The application relates to the technical field of material science and engineering, in particular to a micro deep hole inner coating process and a coating device.
Background
The micro-forming technology, which is a well-known technology for miniaturizing the size of a metal stamping process, has been contributing to the reduction of mass production costs of fine to sub-millimeter precision parts. With the development of device integration, multifunction and miniaturization, improvement of precision of micro devices is required while keeping manufacturing costs low. One of the key technologies to meet these requirements is to increase the life of the tool. In actual production, as the number of products increases, adhesion of the processed material and abrasion of the micro-mold surface cause a significant decrease in its forming accuracy. For example, at the manufacturing site of the microperforation process, typically 10000 times of process are limitations to ensure that the precision of the produced product is in the sub-micron range of pore quality. In addition, since the precise alignment time for positioning the die is a large part of the total operation time at each tool life interval, the improvement of the tool life plays an important role in reducing the production cost. Therefore, even if the manufacturing cost of the micro-mold is higher and higher, it is necessary to develop a high-performance micro-mold to achieve high wear toughness and high adhesion of the working material.
In response to these demands, in the background of rapid development of hard coat for tools, the application of hard coat on a mold substrate targeted for micro-forming is increasingly active. Although application studies in the field of dry micro-molding have been well developed, high-performance micro-molds having utility on an industrial scale have not been developed. Particularly, the traditional hard film deposition process encounters difficulty in depositing high-performance films on the inner wall of a closed special-shaped micro-die with a submillimeter aperture. In order to increase the service life of the tool, it is necessary to uniformly deposit a thin film having high adhesion and high wear resistance and high toughness on a three-dimensional complex-shaped structure.
In view of the non-planar surface uniformity, while CVD processes have greater advantages over PVD processes, film properties and substrate temperature are not suitable for micro-die fabrication. For PVD processes, directional and energy control is achieved by ionizing the vaporized species. Since all PVD deposition techniques lack the ability to cover surfaces that do not face the particle source, especially internal structures such as trenches or holes, it is important to improve the uniformity of film thickness and quality. Especially for micropores with an aspect ratio of 8:1 and larger, no good method for improving the uniformity of the inner wall is available in the industry, the uniformity in the prior art is only about 20% of the uniformity of the film thickness, and in order to achieve the purpose of improving the uniformity, a plurality of devices such as auxiliary cathodes, auxiliary electrodes and the like are often needed to be added, so that the production cost is increased, and the production is very uncomfortable due to the additional device assembly precision and the like.
Disclosure of Invention
The application aims to provide a micro deep hole inner coating process and a coating device, so as to solve the problems.
In order to achieve the above purpose, the application adopts the following technical scheme:
a micro deep hole inner coating process is used for coating a workpiece with a hole and comprises the following steps:
placing the workpiece and the magnetic control target oppositely to enable the workpiece to be in a autorotation state;
carrying out gas ion cleaning on the workpiece;
and (3) coating the workpiece, and performing sputter coating on the workpiece by adopting a high-power pulse magnetron sputtering technology, and completing the deposition of the film layers on the surface of the workpiece and the surface of the side wall of the hole by matching with the high-power pulse bias coupled on the workpiece.
Preferably, before the workpiece and the magnetic control target are placed oppositely, the micro deep hole internal coating process further comprises the step of preprocessing the workpiece, and ultrasonic cleaning is carried out on the workpiece by adopting an organic solvent or deionized water to remove stains on the surface of the workpiece and on the inner side wall of the workpiece hole.
Preferably, the distance between the workpiece and the magnetic control target is 6-20cm.
Preferably, the workpiece rotates at a frequency of 5Hz-30Hz.
Preferably, the step of gas ion cleaning the workpiece comprises: vacuumizing, heating and degassing; argon is filled, a high-frequency high-voltage power supply is used for applying the argon on the substrate, so that the argon is ionized, and the argon ions are utilized to remove oxide layers on the surfaces of the workpiece and the hole wall.
Preferably, the gas ion cleaning is performed on the workpiece for a period of 10-60min.
Preferably, when the workpiece is coated, the power density on the magnetic control target reaches 0.01kw/cm 2 -5kw/cm 2 The frequency is set to 50-1000Hz and the pulse width is set to 50-300 mu s.
Preferably, the power density on the magnetron target is up to 1.5kw/cm 2 The frequency was set to 100Hz and the pulse width 200 mus.
Preferably, the coupling high power pulse bias voltage used on the workpiece is 10 mu s-200 mu s phase difference and 20 mu s-500 mu s pulse width when coating the workpiece.
The utility model provides a coating device for among the above-mentioned little deep hole internal coating process, includes cavity, magnetic control target and work piece revolving rack, the magnetic control target with the work piece revolving rack all set up in the cavity, the work piece revolving rack with the magnetic control target sets up relatively, the work piece revolving rack is used for placing the work piece of waiting to coat film, and drives the work piece rotation, high power pulse voltage is connected to the magnetic control target, coupling high power pulse bias voltage on the work piece revolving rack.
Compared with the prior art, the application has the beneficial effects that:
according to the micro deep hole internal coating process and the coating device, the characteristics of high plasma density and high plasma ionization rate of the high-power pulse magnetron sputtering technology are utilized, a workpiece with a micro hole with a large depth-to-width ratio is placed in front of a magnetron target to rotate, then ions are attracted into the hole by adjusting and controlling a phase difference through coupling bias voltage, so that the hole is in a plasma infiltration state, plasma is deposited on the side wall of the hole, uniformity of a coating film layer on the side wall of the micro hole is effectively improved, and adhesion force of the film layer and quality of the film layer can be improved. In addition, the vacuum coating mode is adopted in the micro deep hole internal coating process, so that the environment pollution can be reduced, and the method is more environment-friendly.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope of the present application.
FIG. 1 is a flow chart of a process for coating a film in a deep hole in a micro-cavity according to embodiment 1 of the present application;
FIG. 2 is a schematic diagram of the high power pulse magnetron sputtering coating in the hole of the workpiece in example 1 of the present application;
FIG. 3 is a schematic diagram of the structure and cross-section of a DC reactive magnetron sputtering (left side) and a high power pulsed magnetron sputtering (right side) used in the present application to deposit a coating in a hole;
FIG. 4 is a schematic diagram showing the deposition rates of the coupling bias HiPIMS and the common bias HiPIMS of the present application for depositing a plating film at different positions in a micro deep hole with a diameter of 1 mm.
Detailed Description
The term as used herein:
"prepared from … …" is synonymous with "comprising". The terms "comprising," "including," "having," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
The conjunction "consisting of … …" excludes any unspecified element, step or component. If used in a claim, such phrase will cause the claim to be closed, such that it does not include materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of … …" appears in a clause of the claim body, rather than immediately following the subject, it is limited to only the elements described in that clause; other elements are not excluded from the stated claims as a whole.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
In these examples, the parts and percentages are by mass unless otherwise indicated.
"parts by mass" means a basic unit of measurement showing the mass ratio of a plurality of components, and 1 part may be any unit mass, for example, 1g may be expressed, 2.689g may be expressed, and the like. If we say that the mass part of the a component is a part and the mass part of the B component is B part, the ratio a of the mass of the a component to the mass of the B component is represented as: b. alternatively, the mass of the A component is aK, and the mass of the B component is bK (K is an arbitrary number and represents a multiple factor). It is not misunderstood that the sum of the parts by mass of all the components is not limited to 100 parts, unlike the parts by mass.
"and/or" is used to indicate that one or both of the illustrated cases may occur, e.g., a and/or B include (a and B) and (a or B).
Embodiments of the present application will be described in detail below with reference to specific examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment provides a process for coating a film on a workpiece with a hole in a micro deep hole, which is used for coating the film on the sidewall of the workpiece in the micro deep hole, so that the uniformity of the film layer of the film coating is good. Solves the problem of uneven film layer when coating film on the side wall of the micropore with large depth-to-width ratio in the prior art. The method is particularly suitable for coating micropores with large depth-to-width ratio (10:1 and above), can be used for depositing hard film layers on complex surfaces of micro-forming cutters, and can also be applied to scenes such as ceramic metallization with complex surface structures including 5G ceramics.
Referring to fig. 1, the process for coating the film in the micro deep hole comprises the following steps:
s101: and placing the workpiece in a coating device, so that the workpiece is opposite to the magnetic control target, and the workpiece is in a autorotation state.
Specifically, a film plating device is provided, a workpiece with micropores is placed opposite to a magnetic control target, so that the workpiece rotates relative to the magnetic control target.
In some embodiments, the coating apparatus comprises a workpiece turret disposed opposite the magnetron target. The workpiece is placed on the workpiece rotating frame and is driven by the workpiece rotating frame to rotate.
The distance between the workpiece placed on the workpiece rotating frame and the magnetic control target is 6-20cm, and the frequency of the workpiece rotating frame driving the workpiece to rotate is 5-30 Hz.
Preferably, in some embodiments, the distance between the workpiece and the magnetic control target is 6-14cm, and the frequency of the workpiece rotating frame driving the workpiece to rotate is 10-20 Hz.
Alternatively, the distance between the workpiece and the magnetron target may be any one of 6cm, 7cm, 8cm, 9cm, 10cm, 11cm, 12cm, 13cm, 14cm, and 6-14cm, and the frequency of rotation may be any one of 10Hz, 12Hz, 15Hz, 17Hz, 20Hz, and 10Hz-20Hz.
In the embodiment, the distance between the workpiece and the magnetic control target is 10cm, and the frequency of the workpiece rotating frame driving the workpiece to rotate is 15Hz.
The workpieces acted in the coating process can be made of different types of materials.
Preferably, the workpiece is made of metal, alloy or stainless steel with good conductivity, and the thickness is 1mm-16mm. The aspect ratio of the holes in the workpiece may be from 1:1 to 16:1, the diameter of the holes can be 0.00001mm-10mm.
S102: and (5) cleaning the workpiece by gas ions.
Specifically, vacuum pumping, heating and argon ion cleaning are sequentially performed by using a coating device.
Vacuumizing the cavity of the coating device to make the vacuum degree of the coating device lower than 5 x 10 -3 Pa, and heating and degassing to enable the temperature in the cavity of the coating device to be 50-500 ℃.
In this embodiment, the vacuum degree of the coating device is 5×10 -3 Pa, the temperature in the cavity of the film plating device is 220 ℃.
Then, argon (Ar) is filled into the cavity of the film plating device, a high-frequency high-voltage bias power supply (2 mu s-10 mu s,40KHz-200 KHz) is applied to the substrate, so that the argon is ionized by 600V, and the argon ions are utilized to remove oxide layers on the surfaces of the workpiece and the hole wall, so that the adhesive force of the subsequent film layer is enhanced.
And (5) carrying out plasma etching cleaning on the workpiece for 10-60min.
S103: and (5) coating the workpiece to finish the deposition of the surface film layers on the side walls of the through holes and the blind holes.
Specifically, a high-power pulse magnetron sputtering technology is adopted, and a coating device is used for carrying out sputtering coating on a microporous workpiece with a large depth-to-width ratio, so that the coating on the surface of the workpiece, the surfaces of the side walls of the through holes and the blind holes is completed.
In some embodiments, the power density on the magnetron target is up to 0.01kw/cm 2 -5kw/cm 2 The frequency is set to 50-1000Hz and the pulse width is set to 50-300 mu s. The work piece is biased by coupling high power pulse with a phase difference of 10 mu s-200 mu s and a pulse width of 20 mu s-500 mu s.
Preferably, the power density on the magnetron target is up to 0.03kw/cm 2 -1.5kw/cm 2 The frequency is set to 50-1000Hz and the pulse width is set to 50-300 mu s. The phase difference of the coupled high-power pulse bias voltage adopted on the workpiece is 20 mu s-150 mu s, and the pulse width is 50 mu s-300 mu s.
In this example, the power density on the magnetron target was 1.5kw/cm 2 The frequency was set to 100Hz and the pulse width 200 mus. The coupled high power pulse bias voltage used on the workpiece has a phase difference of 50 mus and a pulse width of 200 mus.
The uniformity of the coating film on the side wall of the micropore can be effectively improved by regulating and controlling the phase difference of the coupling bias voltage on the workpiece.
Please refer to the figure2, at a vacuum level of less than 5 x 10 -3 Introducing inert gas such as argon into the Pa high vacuum environment, and carrying out 600V glow ionization to enable negative argon ions to be attracted by a cathode target material and bombard the target material; positive atoms on the surface of the target material overflow through collision, move in a vacuum environment and are ejected towards the direction bearing the workpiece; because the high pulse voltage is adopted, the density of the sputtered plasma is extremely high and is more than 1 order of magnitude larger than that of the common direct current sputtering, so that one side of the whole workpiece facing the target direction is in a plasma infiltration state; and because of the characteristic of the high-power pulse magnetron sputtering technology, the ionization rate of particles in the plasma is extremely high and can reach 70% -80%, when the high-density plasma enters the micro deep hole of the workpiece, pulse bias is applied to the workpiece, negative potentials are all present in the micro deep hole in the three-dimensional direction, and positive ions of a target material are attracted to deposit on the three-dimensional surface of the micro deep hole. And the inside of the hole is in a plasma infiltration state, so that the uniformity of the film layer in the hole is good.
Different film layers can be prepared on the workpiece by adopting different targets, for example, a Cr target, a Ti target, a Nb target and a WC target can be selected as the targets, but the targets are not limited to the targets.
In this embodiment, metal Cr is used as a target, stainless steel is selected as a workpiece, and a Cr layer is sputtered on the workpiece.
As shown in fig. 3, a structure and a cross-sectional view of a deposition film in a hole in the prior art direct current reactive magnetron sputtering (DCMS) (left side) and high power pulse magnetron sputtering (HiPIMS) (right side) used in the present embodiment are shown. Compared with direct current reactive magnetron sputtering, the high-power pulse magnetron sputtering adopted by the application can ensure that the uniformity of a deposited film layer is higher, the adhesive force of the film layer is enhanced, and the thickness of a plating film is also increased.
FIG. 4 is a schematic view showing the deposition rates of the deposition films at different positions in the micro deep hole with the diameter of 1mm by coupling the bias HiPIMS and the common bias HiPIMS according to the present application. Compared with the common bias voltage HiPIMS, the coupling bias voltage HiPIMS adopted by the application can improve the deposition speed of the micro deep hole at all positions of the hole depth, and compared with the common bias voltage HiPIMS, the difference value of the deposition speed of the coupling bias voltage HiPIMS film layer at the positions of the hole depth is reduced, so that the uniformity of the film layer is obviously improved.
In some embodiments, before step S101, the micro deep hole in-coating process further includes a step of preprocessing the workpiece: and ultrasonically cleaning the workpiece by adopting an organic solvent or deionized water to remove stains on the surface of the workpiece and on the inner side wall of the workpiece hole.
Specifically, the step of preprocessing the workpiece includes:
1. placing the workpiece into pure water, and removing the residual particulate impurities on the surface of the workpiece and in the through holes and blind holes by using an ultrasonic cleaner;
2. placing the workpiece into acetone, and removing grease impurities attached to the surfaces of the workpiece, the through holes and the blind holes (side walls) by using an ultrasonic cleaner;
3. and (3) putting the workpiece into pure water, performing secondary cleaning by using an ultrasonic cleaner, and drying in an oven.
Wherein, the time length of each ultrasonic cleaner is controlled to be 10-30min, so as to completely remove impurities.
The application fully utilizes the characteristics of high plasma density and high plasma ionization rate of the high-power pulse magnetron sputtering technology, places a workpiece with a micropore with a large aspect ratio in front of a magnetron target to rotate, then attracts ions into the hole by adjusting and controlling a phase difference through coupling bias voltage, so that the hole is in a plasma infiltration state, and the plasma is deposited on the side wall of the hole, thereby not only effectively improving the uniformity of a film coating layer on the side wall of the micropore, but also improving the adhesive force of the film layer and the quality of the film layer. In addition, the vacuum coating mode is adopted in the micro deep hole internal coating process, so that the environment pollution can be reduced, and the method is more environment-friendly.
Example 2
The embodiment provides a coating device which is used for coating a workpiece with holes.
The coating device comprises a cavity, a magnetic control target and a workpiece rotating frame. The magnetic control target and the workpiece rotating frame are arranged in the cavity.
The cavity is used for isolating air and carrying out reaction. The workpiece rotating frame is arranged opposite to the magnetic control target, is used for placing a workpiece to be coated and drives the workpiece to rotate.
The magnetic control target is connected with high-power pulse voltage. The workpiece turret is coupled with a high power pulse bias.
The coating device can coat the workpiece with the holes by using a high-power pulse magnetron sputtering technology. In the side wall of the workpiece micro deep hole, the uniformity of the film layer of the film coating is good.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features but not others included in other embodiments, combinations of features of different embodiments are meant to be within the scope of the application and form different embodiments. For example, in the claims below, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the application and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (8)
1. The process for coating the film on the workpiece with the hole is characterized by comprising the following steps of:
placing the workpiece and the magnetic control target oppositely to enable the workpiece to be in a autorotation state;
carrying out gas ion cleaning on the workpiece;
coating the workpiece, and performing sputter coating on the workpiece by adopting a high-power pulse magnetron sputtering technology, and completing the deposition of the surface film layers on the surface of the workpiece and the surface film layers on the side wall of the hole by matching with the high-power pulse bias coupled on the workpiece;
when the workpiece is coated, the power density on the magnetic control target reaches 0.01kw/cm 2 -5kw/cm 2 The frequency is set to be 50-1000Hz, and the pulse width is set to be 50-300 mu s;
when the workpiece is coated, the coupling high-power pulse bias voltage is used on the workpiece, the phase difference is 10 mu s-200 mu s, and the pulse width is 20 mu s-500 mu s.
2. The process according to claim 1, wherein the process further comprises a step of pretreating the workpiece before the workpiece is placed opposite to the magnetron target, and performing ultrasonic cleaning on the workpiece with an organic solvent or deionized water to remove stains on the surface of the workpiece and on the inner side wall of the workpiece hole.
3. The process of claim 1, wherein the distance between the workpiece and the magnetron target is 6-20cm.
4. The process of claim 1, wherein the workpiece rotates at a frequency of 5Hz to 30Hz.
5. The process of claim 1, wherein the step of cleaning the workpiece with gas ions comprises: vacuumizing, heating and degassing; argon is filled, a high-frequency high-voltage power supply is used for applying the argon on the substrate, so that the argon is ionized, and the argon ions are utilized to remove oxide layers on the surfaces of the workpiece and the hole wall.
6. The process of claim 5, wherein the gas ion cleaning is performed on the workpiece for a period of 10-60 minutes.
7. The process for coating a film in a deep hole according to claim 1, wherein the power density on the magnetron target is 1.5kw/cm 2 The frequency was set to 100Hz and the pulse width 200 mus.
8. The coating device is characterized by comprising a cavity, a magnetic control target and a workpiece rotating frame, wherein the magnetic control target and the workpiece rotating frame are arranged in the cavity, the workpiece rotating frame is opposite to the magnetic control target, the workpiece rotating frame is used for placing a workpiece to be coated and driving the workpiece to rotate, the magnetic control target is connected with high-power pulse voltage, and the workpiece rotating frame is coupled with high-power pulse bias voltage.
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