CN112779494A - Surface metallization process of dielectric ceramic filter - Google Patents
Surface metallization process of dielectric ceramic filter Download PDFInfo
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- CN112779494A CN112779494A CN202011408493.4A CN202011408493A CN112779494A CN 112779494 A CN112779494 A CN 112779494A CN 202011408493 A CN202011408493 A CN 202011408493A CN 112779494 A CN112779494 A CN 112779494A
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- C23C14/02—Pretreatment of the material to be coated
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- 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
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- 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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- 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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- 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
- C23C14/3457—Sputtering using other particles than noble gas ions
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- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/48—Ion implantation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention belongs to the field of nonmetal surface metallization, and particularly relates to a surface metallization process of a dielectric ceramic filter, which comprises the following steps: ultrasonically cleaning a dielectric ceramic filter by using an organic solvent; baking at high temperature and keeping the temperature; then charging into a furnace for vacuumizing, heating and preserving heat; introducing argon gas into the furnace, and starting a Hall ion source to perform sputtering cleaning on the surface of the dielectric ceramic filter; stopping introducing argon, adopting a high-energy pulse ion injection method, adopting a metal target, and injecting metal ions into the surface of the dielectric ceramic filter; adopting a magnetron sputtering method, introducing argon and reducing gas, and adopting a metal target to deposit a metal layer on the surface of the metal layer subjected to ion implantation; and continuously introducing argon, and taking out the medium ceramic filter from the furnace after the medium ceramic filter is cooled. The process can effectively improve the film-substrate binding force between the ceramic substrate and the surface metal conductive coating, so that the metallized dielectric ceramic filter has good electrical property.
Description
Technical Field
The invention belongs to the field of nonmetal surface metallization, and particularly relates to a surface metallization process of a dielectric ceramic filter.
Background
When a communication system selects a channel, a receiving end should have a signal-to-noise ratio as high as possible, and a transmitting end should generate interference as little as possible in adjacent frequency bands, so that a high-performance filter and a resonator are essential. As such, microwave filters that can perform signal frequency selection and noise removal functions are increasingly important in increasingly crowded frequency spectrum ranges and in more complex electromagnetic environments. The typical base station filter is a dielectric resonant cavity filter, which is different from a traditional metal cavity filter, the dielectric resonant cavity filter is made by loading a dielectric resonant cavity with a microwave dielectric ceramic material with a certain dielectric constant, and the surface of the dielectric resonant cavity needs to be metallized to make the dielectric resonant cavity conductive, so that the dielectric resonant cavity can replace metal materials.
At present, a 5G dielectric ceramic filter is generally prepared by using a silver paste soaking coating or spraying blade coating method, however, the prepared coating is not strong in adhesive force and difficult to meet the process requirement, repeated sintering treatment is required, the required silver amount of the preparation method is large, the silver content requirement of the silver paste is high and needs to reach 80-90%, the silver paste is large in loss amount and needs to depend on import, so that the overall cost of the 5G dielectric ceramic filter is greatly increased, and the method is not beneficial to environmental protection and resource utilization.
The alternatives currently sought are mainly hybrid plating methods, such as electroless plating plus electroplating, and magnetron sputtering. However, the hybrid plating method has a serious wastewater treatment problem, is greatly limited by the plating solution, and is easy to generate bubbles or film-substrate separation at high temperature or under large current; the traditional magnetron sputtering method also has the problems of insufficient film adhesion and high process cost.
Therefore, it is urgently needed to develop a new surface metallization process of a dielectric ceramic filter, which can effectively improve the film-substrate bonding force between the ceramic substrate and the surface metal conductive coating and reduce the production cost.
Disclosure of Invention
The invention aims to provide a surface metallization process of a dielectric ceramic filter, which can effectively improve the film-substrate bonding force between a ceramic substrate and a surface metal conductive coating and ensure that the metallized dielectric ceramic filter has good electrical property.
The technical scheme for realizing the purpose of the invention is as follows: a process for surface metallization of a dielectric ceramic filter, the method comprising the steps of:
step (1), ultrasonically cleaning a dielectric ceramic filter by using an organic solvent;
step (2), baking the medium ceramic filter subjected to ultrasonic cleaning at high temperature and preserving heat;
step (3), charging the dried dielectric ceramic filter into a furnace, and carrying out vacuumizing, heating and heat preservation treatment;
introducing argon gas into the furnace, and starting a Hall ion source to perform sputtering cleaning on the surface of the dielectric ceramic filter;
stopping introducing argon, adopting a high-energy pulse ion injection method, adopting a metal target, and injecting metal ions into the surface of the dielectric ceramic filter;
step (6), introducing argon and reducing gas by adopting a magnetron sputtering method, and depositing a metal layer on the surface of the ion-implanted metal layer by adopting a metal target;
and (7) continuously introducing argon, and taking out the dielectric ceramic filter from the furnace after the dielectric ceramic filter is cooled.
Further, the organic solvent in the step (1) is acetone and absolute ethyl alcohol.
Further, the baking temperature in the step (2) is 200 ℃, and the baking time is 2 hours; the heat preservation temperature is 80 ℃, and the heat preservation time is 8 hours.
Further, the vacuum degree of the vacuum pumping in the step (3) is 1 × 10-3Pa; the heating temperature is 150 ℃, and the heat preservation time is 30 min.
Further, before argon is introduced into the furnace in the step (4), the vacuum degree is maintained to be 9 x 10-4Pa。
Further, the vacuum degree during sputtering cleaning in the step (4) is 7-9 multiplied by 10-3Pa, parameters of the hall ion source are: voltage: 1000V-1500V, current: 0.3A-1.0A, duty cycle: 20-50% and the sputtering cleaning time is 40 min.
Further, the high energy pulse in the step (5)When the impact ions are injected, the purity of the metal ions of the metal target is 99.99%, and the working air pressure is 4-8 multiplied by 10-4Pa, an implantation voltage of 26-32 kv, and an implantation dose of 7.2 × 1017ions/cm2～2.4×1018ions/cm2The injection time is 20min-40 min.
Further, the metal in the step (5) is Ag, Cu, Ti or Ni.
Further, in the step (6), during magnetron sputtering, the purity of metal ions of the metal target is 99.99%, and the vacuum degree is 6-8 × 10-4Pa, the working pressure is 0.1-0.5 Pa, the sputtering power is 1500-2400W, the thickness is 8-10 μm, and the time for depositing the metal layer is 20 min.
Further, the metal in the step (6) is Ag or Cu.
Further, the volume ratio of the argon gas to the reducing gas in the step (6) is 3: 1, the purity of the argon and the reducing gas are both 99.99 percent.
Further, the reducing gas in the step (6) is CO and H2S or CH4。
The invention has the beneficial technical effects that:
1. according to the surface metallization process of the dielectric ceramic filter, the reducing gas is introduced when the metal layer is deposited, so that adsorbed oxygen can be effectively removed, the oxidation probability of the metal layer is reduced, and the bonding force of the metal layer on the ceramic substrate is improved; when the metal layer is prepared, the addition of reducing gas effectively simplifies the preparation step of the intermediate layer between the injection layer and the metal layer in the conventional process means; one interface is reduced, the loss in the signal transmission process is reduced, and the working performance of the filter is improved;
2. the surface metallization process of the dielectric ceramic filter disclosed by the invention can effectively simplify the treatment process, shorten the process time, reduce the cost and lay a good foundation for industrial application by removing the intermediate layer in the conventional process means;
3. according to the surface metallization process of the dielectric ceramic filter, the dielectric ceramic filter is ultrasonically cleaned by using the organic solvent, organic matters and attached impurities on the surface of the ceramic can be effectively removed, and the surface cleanliness is improved;
4. according to the surface metallization process of the dielectric ceramic filter, impurity gas and water molecules adsorbed by the ceramic material can be effectively removed through high-temperature baking (the ceramic material is of a porous structure and is easy to adsorb gas in the air), and the metal coating is effectively prevented from being oxidized;
5. in the surface metallization process of the dielectric ceramic filter, the sputtering cleaning bombards the surface of a workpiece by ionized argon ions, so that particles attached to the surface of the workpiece and some impurity molecules adsorbed in pores can be further removed; on the other hand, the surface activity and the wettability of the dielectric ceramic filter workpiece can be effectively improved, and the bonding force between the substrate and the surface prepared metal layer can be directly improved;
6. according to the high-energy pulse ion implantation method in the surface metallization process of the dielectric ceramic filter, metal ions such as Ag, Cu, Ti, Ni and the like are implanted into the surface of a workpiece of the dielectric ceramic filter, so that on one hand, the effect of filling pores can be achieved, on the other hand, a base point can be provided for combination with a surface conductive metal layer, the effect of buffer transition is achieved for combination of a substrate and the surface metal layer, and the binding force is remarkably improved.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1 with BaTi4O9Surface metallization of dielectric ceramic filters as substrates
Step (1) mixing BaTi4O9Immersing the ceramic block workpiece in acetone for ultrasonic cleaning for 20min, drying, and immersing in absolute ethyl alcohol for ultrasonic cleaning for 20 min;
drying the ceramic block workpiece subjected to ultrasonic cleaning, then placing the ceramic block workpiece into a muffle furnace to bake for 2 hours at 200 ℃, and then preserving heat for 8 hours at 80 ℃ for later use;
step (3), the ceramic block workpiece is vacuumized after being charged in a furnace, and the vacuum degree is 1 multiplied by 10-3After Pa, a heating power supply is started, the ceramic block workpiece rotates in a continuous revolution mode, the heating temperature is set to be 150 ℃, and the temperature reachesKeeping the temperature at 150 ℃ for 30min, removing air adsorbed on the inner wall of the vacuum chamber, and improving the vacuum degree;
step (4), the vacuum degree enters 9 multiplied by 10-4Introducing argon after Pa, starting a Hall ion source to perform sputtering cleaning on the surface of the ceramic block workpiece, and maintaining the vacuum degree at 8 x 10-3Pa, parameters of the hall ion source are: the voltage is 1500V, the current is 0.5A, the duty ratio is 20%, and the time is 40 min;
and (5) stopping introducing argon, implanting Ti ions into the surface of the ceramic block workpiece by using a high-energy pulse ion implantation method and adopting a Ti target, wherein the purity of the Ti ions of the adopted Ti target is 99.99%, and the working air pressure is 8 multiplied by 10-4Pa, implant voltage of 28kv, implant dose of 9 × 1017ions/cm2The injection time is 20 min;
after the ion implantation process is finished, starting to adopt a magnetron sputtering method, adopting a Cu target, and preparing a Cu layer on the surface of the ion implantation Ti layer, wherein the purity of Cu ions of the adopted Cu target is 99.99%, and the background vacuum degree is 6 multiplied by 10-4Pa, introducing argon and CH4Gas, volume ratio 3: 1, argon and CH4The gas purity of the gas is 99.99 percent, the working pressure is 0.1Pa, the sputtering power is 2100W, the thickness is 10 mu m, and the time for depositing the Cu layer is 20 min;
and (7) continuously introducing argon, and taking out the workpiece and storing the workpiece in a vacuum drying environment when the temperature is reduced to below 50 ℃.
Through the steps of BaTi4O9A metal Cu layer with the thickness of 10 mu m is prepared on the surface of the dielectric ceramic filter which is taken as a substrate. The bonding force of the metal layer film substrate is tested by a drawing method, and the bonding force of the process film substrate without adding reducing gas is less than 10N/mm2The binding force of the process film base added with reducing gas is more than 20N/mm2. And testing the whole insertion loss of the device, wherein the whole insertion loss of the device added with reducing gas is reduced by more than 20%.
Example 2 with (Zr, Sn) TiO4Surface metallization of dielectric ceramic filters as substrates
Step (1) preparing (Zr, Sn) TiO4Immersing the ceramic block workpiece in acetone for ultrasonic cleaning for 20min,after drying, immersing the fabric in absolute ethyl alcohol for ultrasonic cleaning for 20 min;
drying the ceramic block workpiece subjected to ultrasonic cleaning, then placing the ceramic block workpiece into a muffle furnace to bake for 2 hours at 200 ℃, and then preserving heat for 8 hours at 80 ℃ for later use;
step (3), the ceramic block workpiece is vacuumized after being charged in a furnace, and the vacuum degree is 1 multiplied by 10-3After Pa, a heating power supply is started, the rotation mode of the ceramic block workpiece is continuous revolution, the heating temperature is set to be 150 ℃, the temperature is kept for 30min after reaching 150 ℃, air adsorbed on the inner wall of the vacuum chamber is removed, and the vacuum degree is improved;
step (4), the vacuum degree enters 9 multiplied by 10-4Introducing argon after Pa, starting a Hall ion source to perform sputtering cleaning on the surface of the ceramic block workpiece, and maintaining the vacuum degree at 9 x 10-3Pa, parameters of the hall ion source are: the voltage is 1000V, the current is 1.0A, the duty ratio is 50%, and the time is 20 min;
and (5) stopping introducing argon, implanting Ni ions into the surface of the ceramic block workpiece by using a high-energy pulse ion implantation method and adopting a Ni target, wherein the purity of the Ni ions of the adopted Ni target is 99.99%, and the working air pressure is 4 multiplied by 10-4Pa, implant voltage of 32kv, and implant dose of 2.4 × 1018ions/cm2The injection time is 40 min;
after the ion implantation process is finished, preparing an Ag layer on the surface of the ion implantation Ni layer by adopting an Ag target by adopting a magnetron sputtering method, wherein the purity of Ag ions of the Ag target is 99.99%, and the background vacuum degree is 6 multiplied by 10-4Pa, introducing argon and CO gas in a volume ratio of 3: 1, the gas purity of argon and CO gas is 99.99%, the working pressure is 0.5Pa, the sputtering power is 1500W, the thickness is 8 μm, and the time for depositing an Ag layer is 20 min;
and (7) continuously introducing argon, and taking out the workpiece and storing the workpiece in a vacuum drying environment when the temperature is reduced to below 50 ℃.
Through the steps in (Zr, Sn) TiO4And preparing a metal Ag layer with the thickness of 8 mu m on the surface of the dielectric ceramic filter serving as the substrate. The bonding force of the metal layer film substrate is tested by a drawing method, and the bonding force of the process film substrate without adding reducing gas is less than 10N/mm2The binding force of the process film base added with reducing gas is more than 25N/mm2. And testing the whole insertion loss of the device, wherein the whole insertion loss of the device added with reducing gas is reduced by more than 15%.
The present invention has been described in detail with reference to the embodiments, but the present invention is not limited to the embodiments, and various changes can be made without departing from the gist of the present invention within the knowledge of those skilled in the art. The prior art can be adopted in the content which is not described in detail in the invention.
Claims (12)
1. A process for metallizing a surface of a dielectric ceramic filter, said process comprising the steps of:
step (1), ultrasonically cleaning a dielectric ceramic filter by using an organic solvent;
step (2), baking the medium ceramic filter subjected to ultrasonic cleaning at high temperature and preserving heat;
step (3), charging the dried dielectric ceramic filter into a furnace, and carrying out vacuumizing, heating and heat preservation treatment;
introducing argon gas into the furnace, and starting a Hall ion source to perform sputtering cleaning on the surface of the dielectric ceramic filter;
stopping introducing argon, adopting a high-energy pulse ion injection method, adopting a metal target, and injecting metal ions into the surface of the dielectric ceramic filter;
step (6), introducing argon and reducing gas by adopting a magnetron sputtering method, and depositing a metal layer on the surface of the ion-implanted metal layer by adopting a metal target;
and (7) continuously introducing argon, and taking out the dielectric ceramic filter from the furnace after the dielectric ceramic filter is cooled.
2. The process of claim 1, wherein the organic solvent used in step (1) is acetone or absolute ethanol.
3. The process of claim 1, wherein in the step (2), the baking temperature is 200 ℃ and the baking time is 2 h; the heat preservation temperature is 80 ℃, and the heat preservation time is 8 hours.
4. The process of claim 1, wherein the degree of vacuum applied in step (3) is 1 x 10-3Pa; the heating temperature is 150 ℃, and the heat preservation time is 30 min.
5. The process of claim 1, wherein the step (4) of maintaining the degree of vacuum of 9 x 10 before introducing argon gas into the furnace is performed-4Pa。
6. The process of claim 1, wherein the degree of vacuum in the step (4) of sputter cleaning is 7 to 9 x 10-3Pa, parameters of the hall ion source are: voltage: 1000V-1500V, current: 0.3A-1.0A, duty cycle: 20-50% and the sputtering cleaning time is 40 min.
7. The process of claim 1, wherein in the step (5), when the high-energy pulse ions are implanted, the purity of the metal ions of the metal target is 99.99%, and the working gas pressure is 4-8 x 10- 4Pa, an implantation voltage of 26-32 kv, and an implantation dose of 7.2 × 1017ions/cm2～2.4×1018ions/cm2The injection time is 20min-40 min.
8. The process of claim 7, wherein the metal in step (5) is Ag, Cu, Ti or Ni.
9. A process for metallizing a surface of a dielectric ceramic filter according to claim 1, further characterized in that said step (6) is carried outDuring magnetron sputtering, the purity of metal ions of the metal target is 99.99%, and the vacuum degree is 6-8 multiplied by 10-4Pa, the working pressure is 0.1-0.5 Pa, the sputtering power is 1500-2400W, the thickness is 8-10 μm, and the time for depositing the metal layer is 20 min.
10. The process of claim 9, wherein the metal in step (6) is Cu or Ag.
11. The process of claim 1, wherein the volume ratio of argon gas to reducing gas in step (6) is 3: 1, the purity of the argon and the reducing gas are both 99.99 percent.
12. The process of claim 11, wherein the reducing gas in step (6) is CO or H2S or CH4。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113802104A (en) * | 2021-08-10 | 2021-12-17 | 深圳戴尔蒙德科技有限公司 | Preparation method of metal layer of ceramic dielectric filter |
| CN113896568A (en) * | 2021-09-03 | 2022-01-07 | 摩比天线技术（深圳）有限公司 | Composite dielectric ceramic, preparation method thereof and microwave filter |
| CN114592176A (en) * | 2021-12-31 | 2022-06-07 | 核工业西南物理研究院 | Ion implantation method for replacing metal transition connection layer |
| CN115819120A (en) * | 2022-12-05 | 2023-03-21 | 广州天极电子科技股份有限公司 | Pretreatment method of ceramic substrate and method for coating ceramic substrate |
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