CN112695305A - Preparation method of high-binding-force electroplated film ceramic resistor - Google Patents
Preparation method of high-binding-force electroplated film ceramic resistor Download PDFInfo
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- CN112695305A CN112695305A CN202011465574.8A CN202011465574A CN112695305A CN 112695305 A CN112695305 A CN 112695305A CN 202011465574 A CN202011465574 A CN 202011465574A CN 112695305 A CN112695305 A CN 112695305A
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- force
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- electroplated film
- ceramic resistor
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1689—After-treatment
- C23C18/1692—Heat-treatment
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
Abstract
The invention discloses a preparation method of a high-binding force electroplated film ceramic resistor, which comprises the following steps: before electroplating, degreasing treatment is carried out, usually gasoline or alcohol is used for cleaning, and then chemical degreasing is carried out; step two, coarsening: coarsening the surface of the deoiled ceramic product by adopting a chemical etching coarsening method; step three, sensitization: adsorbing a layer of divalent tin ions with reducibility on the roughened part surface, and reducing palladium ions into palladium with catalytic action during subsequent ion activation treatment, wherein the step four is activation treatment: forming a layer of noble metal layer with catalytic activity on the surface of the part, and spontaneously performing chemical plating, wherein the step five is reduction: changing the catalytic activity of the surface of the part, and adopting the water plating and heat treatment process to prepare the high-binding-force electroplated film ceramic resistor.
Description
Technical Field
The invention relates to the technical field of ceramic resistors, in particular to a preparation method of a high-binding-force electroplated film ceramic resistor.
Background
The metal film resistor is a resistor which takes special metal or alloy as resistance material and basically forms a resistance film layer on ceramic by a vacuum evaporation or sputtering method. Such resistors are typically made by a vacuum evaporation process, i.e. heating the alloy in a vacuum, evaporating the alloy, depositing it on the surface of the ceramic rod to form a conductive metal film. The resistance can be controlled by notching and changing the thickness of the metal film. The metal film resistor has flexible manufacture process, and can be used to adjust its material composition and film thickness, and to adjust resistance value by grooving, so as to obtain resistor with good performance and wide resistance range.
The existing metal film preparation method is to put the ceramic rod in the rotating disk of the physical vapor deposition cavity, and rotate the product by the rotation of the rotating disk, so that the surface of the magnetic rod is uniformly covered with 0.2um nickel metal film, as shown in the attached figure 1 of the specification.
PVD is a Physical Vapor Deposition (Physical Vapor Deposition) technique, which is a technique for vaporizing a material (commonly called a target or a film) into gaseous molecules, atoms or ions by a Physical method under vacuum and depositing the gaseous molecules, atoms or ions on a workpiece to form a thin film with a specific function.
The metal film deposited by PVD vapor deposition is combined with the magnetic bar through Van der Waals force, the binding force is low, the metal film can be adhered by a transparent adhesive tape, so that the defects that the metal film is locally peeled off and the like easily occur during subsequent finished product processing, and the preparation of a precise ceramic resistor is not facilitated.
Disclosure of Invention
The invention aims to provide a preparation method of a high-bonding-force electroplated film ceramic resistor, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-bonding-force electroplated film ceramic resistor comprises the following steps:
step one, oil removal: before electroplating, degreasing treatment is carried out, usually gasoline or alcohol is used for cleaning, and then chemical degreasing is carried out;
step two, coarsening: coarsening the surface of the deoiled ceramic product by adopting a chemical etching coarsening method to improve the surface hydrophilicity and form proper roughness of the ceramic product so as to ensure that the plating layer has good adhesive force;
step three, sensitization: adsorbing a layer of divalent tin ions with reducibility on the surface of the coarsened part, and reducing palladium ions into palladium with catalytic action during subsequent ion type activation treatment;
step four, activation treatment: forming a noble metal layer with catalytic activity on the surface of the part, so that chemical plating can be carried out spontaneously;
step five, reduction: changing the catalytic activity of the surface of the part, removing the activating solution remained on the surface of the part and preventing the activating solution from being brought into the chemical plating solution to cause solution decomposition;
step six, chemical nickel plating: the palladium particles on the surface of the ceramic rod catalyze the chemical nickel reaction to form a compact film layer on the surface;
step seven, heat treatment: the chemical nickel layer with microscopic microporous surface is heat treated to volatilize residual water and strengthen the corrosion resistance of the product.
Preferably, the chemical degreasing liquid in the step one comprises the following components and process conditions:
preferably, the chemical etching coarsening process described in step two is as follows:
| hydrofluoric acid | 50-60mL/L |
| Ammonium fluoride | 200-220g/L |
| Time | 8-10min |
| Temperature of | 30℃ |
Preferably, the sensitization process described in step three is as follows:
preferably, the activation treatment process described in step four is as follows:
preferably, the reduction process in step five is as follows:
| H2SO4 | 35-45g/l |
| dispergation salt | 18-22g/L |
| Time | 5-10s |
| Temperature of | At room temperature |
Preferably, the chemical nickel plating treatment process in the sixth step is as follows:
| NiSO4.6H2O | 15-22g/l |
| PH | 8.0-8.5 |
| NaH2PO2 | 5.0-8.0g/l |
| Na3Cit | 30-40g/l |
| NH4Cl | 30-38g/l |
| NiSO4.6H2O | 15-22g/l |
| NaH2PO2 | 5.0-8.0g/l |
| PH | 8.0-8.5 |
| Time | 8–10min |
| temperature of | At room temperature |
Preferably, in the heat treatment process in the seventh step, the heating speed of the heating roller is set to be 5 ℃/min, the temperature is increased to 400 ℃, the rotating speed of the single roller is 10 revolutions per minute, and the heat is preserved for 3 hours.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the water plating and heat treatment process, the nickel plating film has uniform appearance, no shedding, good bonding force of the film layer, good compactness of the film layer and better performance of the film layer.
Drawings
FIG. 1 is a diagram of a ceramic rod produced by a conventional metal film production method;
FIG. 2 is a diagram of the resistance of the metal film formed by the water-plating and heat treatment process according to the present invention;
FIG. 3 is a schematic view of the overall process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-3, the present invention provides a technical solution: a preparation method of a high-bonding-force electroplated film ceramic resistor comprises the following steps:
step one, oil removal: the surface of the ceramic product is always stained with oil stain and hand sweat, which can lead the adhesion of the electroplated layer to be poor and generate cracking, bubbling and falling off, the oil removal treatment is carried out before electroplating, usually gasoline or alcohol is used for cleaning, then chemical oil removal is carried out, and the components and the process conditions of the chemical oil removal liquid are as follows;
step two, coarsening: the coarsening method is a most critical process for determining the adhesive force of the plating layer, and has various coarsening methods and different effects, and the coarsening by chemical etching is superior to the coarsening by solvent swelling and the coarsening by mechanical etching in terms of improving the adhesive force of the plating layer;
| hydrofluoric acid | 50-60mL/L |
| Ammonium fluoride | 200-220g/L |
| Time | 8-10min |
| Temperature of | 30℃ |
Step three, sensitization: the ceramic product is an insulator, can not be directly electroplated, and needs to be sensitized, activated and chemically plated before electroplating, wherein the mechanism of sensitization treatment is to make the roughened surface of the part adsorb a layer of divalent tin ions with reducibility so as to reduce palladium ions into palladium with catalytic action during subsequent ionic activation treatment, and the practical process of sensitization treatment is as follows;
step four, activation treatment: forming a noble metal layer with catalytic activity on the surface of the part, so that chemical plating can be carried out spontaneously;
| PdCl2 | 30-50ppm |
| HCl | 250-300ml/l |
| SnCl2.2H2O | 1-3g/l |
| Time | 10–15s |
| temperature of | At room temperature |
Step five, reduction: through reduction treatment, on one hand, the catalytic activity of the surface can be improved, the chemical plating deposition speed is accelerated, and on the other hand, the activating solution remained on the surface of the part can be removed, so that the activating solution is prevented from being brought into the chemical plating solution to cause solution decomposition;
| H2SO4 | 35-45g/l |
| dispergation salt | 18-22g/L |
| Time | 5-10s |
| Temperature of | At room temperature |
Step six, chemical nickel plating: the palladium particles on the surface of the ceramic rod catalyze the chemical nickel reaction to form a compact film layer on the surface, and the thickness of the film layer is mainly determined by time;
| NiSO4.6H2O | 15-22g/l |
| PH | 8.0-8.5 |
| NaH2PO2 | 5.0-8.0g/l |
| Na3Cit | 30-40g/l |
| NH4Cl | 30-38g/l |
| NiSO4.6H2O | 15-22g/l |
| NaH2PO2 | 5.0-8.0g/l |
| PH | 8.0-8.5 |
| Time | 8–10min |
| temperature of | At room temperature |
Step seven, heat treatment: and seventhly, drying the surface of the ceramic rod by using a heat treatment process to volatilize residual moisture and enhance the corrosion resistance of the product, wherein in the heat treatment process, the heating speed of the heating roller is set to be 5 ℃/min, the temperature is increased to 400 ℃, the rotating speed of the single roller is 10 r/min, and the temperature is kept for 3 hours.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of a high-bonding-force electroplated film ceramic resistor is characterized by comprising the following steps:
step one, oil removal: before electroplating, degreasing treatment is carried out, usually gasoline or alcohol is used for cleaning, and then chemical degreasing is carried out;
step two, coarsening: coarsening the surface of the deoiled ceramic product by adopting a chemical etching coarsening method to improve the surface hydrophilicity and form proper roughness of the ceramic product so as to ensure that the plating layer has good adhesive force;
step three, sensitization: adsorbing a layer of divalent tin ions with reducibility on the surface of the coarsened part, and reducing palladium ions into palladium with catalytic action during subsequent ion type activation treatment;
step four, activation treatment: forming a noble metal layer with catalytic activity on the surface of the part, so that chemical plating can be carried out spontaneously;
step five, reduction: changing the catalytic activity of the surface of the part, removing the activating solution remained on the surface of the part and preventing the activating solution from being brought into the chemical plating solution to cause solution decomposition;
step six, chemical nickel plating: the palladium particles on the surface of the ceramic rod catalyze the chemical nickel reaction to form a compact film layer on the surface;
step seven, heat treatment: the chemical nickel layer with microscopic microporous surface is heat treated to volatilize residual water and strengthen the corrosion resistance of the product.
2. The method for preparing a high-bonding-force electroplated film ceramic resistor as claimed in claim 1, wherein: the chemical degreasing liquid in the step one comprises the following components and process conditions:
3. the method for preparing a high-bonding-force electroplated film ceramic resistor as claimed in claim 2, wherein: the chemical etching coarsening process in the step two is as follows:
4. The method for preparing a high-bonding-force electroplated film ceramic resistor as claimed in claim 1, wherein: the sensitization treatment process in the third step is as follows:
5. the method for preparing a high-bonding-force electroplated film ceramic resistor as claimed in claim 1, wherein: the activation treatment process in the fourth step is as follows:
6. the method for preparing a high-bonding-force electroplated film ceramic resistor as claimed in claim 1, wherein: the reduction process in the fifth step is as follows:
7. The method for preparing a high-bonding-force electroplated film ceramic resistor as claimed in claim 1, wherein: the chemical nickel plating treatment process in the sixth step is as follows:
8. the method for preparing a high-bonding-force electroplated film ceramic resistor as claimed in claim 1, wherein: and seventhly, in the heat treatment process, the heating speed of the heating roller is set to be 5 ℃/min, the heating temperature is increased to 400 ℃, the rotating speed of the single roller is 10 revolutions per minute, and the heat is preserved for 3 hours.
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| CN202011465574.8A CN112695305A (en) | 2020-12-13 | 2020-12-13 | Preparation method of high-binding-force electroplated film ceramic resistor |
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| CN202011465574.8A CN112695305A (en) | 2020-12-13 | 2020-12-13 | Preparation method of high-binding-force electroplated film ceramic resistor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113818061A (en) * | 2021-09-23 | 2021-12-21 | 镇江锦兴表面工程技术有限公司 | Surface electroplating process for ceramic product |
| CN113860919A (en) * | 2021-09-25 | 2021-12-31 | 麦德美科技（苏州）有限公司 | Chemical roughening and metalizing process for alumina ceramic |
| CN115322014A (en) * | 2022-09-14 | 2022-11-11 | 东华大学 | Ceramic substrate with metal coating and preparation method thereof |
| CN115474345A (en) * | 2022-09-14 | 2022-12-13 | 东华大学 | Method for manufacturing ceramic fabric circuit based on screen printing and chemical deposition |
| CN117510097A (en) * | 2023-12-29 | 2024-02-06 | 核工业西南物理研究院 | Silicon-based ceramic surface metallization method and application |
-
2020
- 2020-12-13 CN CN202011465574.8A patent/CN112695305A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113818061A (en) * | 2021-09-23 | 2021-12-21 | 镇江锦兴表面工程技术有限公司 | Surface electroplating process for ceramic product |
| CN113860919A (en) * | 2021-09-25 | 2021-12-31 | 麦德美科技（苏州）有限公司 | Chemical roughening and metalizing process for alumina ceramic |
| CN115322014A (en) * | 2022-09-14 | 2022-11-11 | 东华大学 | Ceramic substrate with metal coating and preparation method thereof |
| CN115474345A (en) * | 2022-09-14 | 2022-12-13 | 东华大学 | Method for manufacturing ceramic fabric circuit based on screen printing and chemical deposition |
| CN117510097A (en) * | 2023-12-29 | 2024-02-06 | 核工业西南物理研究院 | Silicon-based ceramic surface metallization method and application |
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