CN111302834B - Microwave magnetron insulating ceramic ring - Google Patents
Microwave magnetron insulating ceramic ring Download PDFInfo
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Abstract
The invention provides a microwave magnetron insulating ceramic ring, which comprises an annular ceramic base body and metallization layers at two ends of the annular ceramic base body; the processing method of the metallization layer comprises the following steps: s1, preparing a plating assistant agent; s2, processing a high-purity aluminum block and a high-purity copper block; s3, pretreatment: soaking the annular ceramic matrix in the hot plating assistant for 10-20min, and taking out for later use; s4, single-side hot-dip aluminum plating and copper alloy plating; s5, hot-dip aluminizing and copper alloy on two sides; s6, side wall cleaning; s7, electroplating a nickel layer; and S8, cleaning the side wall again. The invention adopts the reasonable matching technology of hot dip aluminum copper alloy and ceramic crystal phase particles, so that the metalized aluminum copper alloy layer can form tight combination with the ceramic body during sintering, and then a metalized nickel layer is plated on the metalized aluminum copper alloy layer, thereby greatly improving the surface quality and tensile strength of the ceramic metalized layer and prolonging the service life of the magnetron.
Description
Technical Field
The invention relates to the technical field of material manufacturing, in particular to a microwave magnetron insulating ceramic ring.
Background
The magnetron features high output power, high efficiency, low working voltage (relative to linear microwave injection tube), small size, light weight and low cost. With the development of science and technology, magnetrons are widely used in the fields of electronics, electric power, chemical industry and the like, and the demand of metallized ceramics, which is one of the core components of magnetrons, tends to increase year by year. At present, in the process of ceramic metallization, because the granularity of metallization powder is too fine, the surface energy is increased, the powder is not easy to disperse, and the flatness and the consistency of a metallization layer are influenced. The excessive granularity of the metallized powder reduces the surface energy, increases the sintering temperature, influences the sintering quality at a given temperature, and causes adverse effect on the combination of a metallized layer and a ceramic layer. In addition, the wall thickness of the existing magnetron ceramic is generally 1.65mm, and the phenomenon that the ceramic wall is broken down or cracks are generated due to overlarge current generated by a magnetic field in the magnetron, so that the service life of the magnetron is influenced.
The traditional microwave magnetron insulating ceramic ring mainly comprises a vacuum evaporation coating method, a vacuum sputtering coating method, a Mo-Mn sintering method and the like, however, the wetting angle of liquid metal on the surface of the ceramic is large, so that the ceramic is not easy to be effectively wetted. The concrete expression is as follows: the ceramic is internally composed of ionic bonds, covalent bonds and a mixture of the ionic bonds and the covalent bonds, and the metal is composed of metal bonds. The reaction between the two is difficult to occur, so that the metal is difficult to form effective wetting on the surface of the ceramic. Secondly, the metal is not easy to be effectively diffused on the surface of the ceramic, and the metal and the ceramic are difficult to be dissolved in solid solution. And thirdly, the difference between the thermal expansion coefficient and the thermal conductivity of the two materials is too large, so that the joint surface of the two materials has larger residual stress in the metallization process. Therefore, it is difficult to directly and effectively bond the two, and these methods cannot achieve a uniform metallized coating on the pore walls of the ceramic.
Disclosure of Invention
The invention aims to provide a microwave magnetron insulating ceramic ring, wherein a metallized nickel layer is plated on a metallized aluminum-copper alloy layer, so that the surface quality and tensile strength of the metallized ceramic layer are greatly improved, the metal layer is uniform and fine, the wall thickness of the ceramic metal layer is effectively improved, the phenomenon that the ceramic wall is broken down or cracks are generated due to overlarge current generated by a magnetic field in the magnetron is avoided, and the service life of the magnetron is prolonged.
The technical scheme of the invention is realized as follows:
the invention provides a microwave magnetron insulating ceramic ring, which comprises the following steps:
s1, preparing the plating assistant agent: the plating assistant agent comprises NH4Cl、NaF、K2ZrF6Cerium chloride, lanthanum chloride and water, and the raw materials are uniformly mixed according to a proportion for later use;
s2, processing the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the grease on the surface by using an ethanol solution, removing an oxide film on the surface by using a hot NaOH solution, finally cleaning by using deionized water, and then putting into an oven for drying;
s3, pretreatment: soaking the annular ceramic matrix in the hot plating assistant for 10-20min, and taking out for later use;
s4, hot-dip aluminum plating, copper alloy: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing the furnace body by using an organic silicon sealant, starting to heat the furnace body until the temperature is set after the sealant is dried, simultaneously introducing high-purity nitrogen with a certain flow rate, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed after the aluminum and the copper in the graphite crucible are melted, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate out together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, and thus obtaining a layer of uniform aluminum-copper alloy film with the thickness of 3-10 microns on the surface of;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; putting the end face of the ring-shaped ceramic substrate which is metalized upwards into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block which are cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat until the set temperature is reached after the sealant is dried, simultaneously introducing high-purity nitrogen with a certain flow rate, pushing the ring-shaped ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed after the aluminum and the copper in the graphite crucible are melted, contacting the ring-shaped ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the ring-shaped ceramic substrate out together with the aluminum-copper alloy liquid attached to the surface and gradually cooling to obtain double-sided metalized ring-shaped ceramic, wherein the metalized layer is a uniform aluminum-copper alloy film with the thickness of 3;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum-copper alloy films of the inner side wall and the outer side wall by using an electric-shock method, and then putting the aluminum-copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece;
s7, nickel layer electroplating: soaking the metallized ceramic piece obtained in the step S6 in nickel electroplating solution for electroplating;
s8, cleaning the side wall again: mechanically polishing the inner side wall and the outer side wall of the metalized ceramic piece electroplated in the step S7 again, wherein the surface roughness Ra is 0.1-0.3 micrometer; and then putting the ceramic ring into deionized water for ultrasonic cleaning for 10-15min to obtain the microwave magnetron insulating ceramic ring.
As a further improvement of the invention, the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)470-120 parts of Cl, 0.5-1.5 parts of NaF and K2ZrF670-120 parts of cerium chloride, 0.01-0.1 part of lanthanum chloride and 500 parts of water 300-.
As a further improvement of the invention, in the step S2, the mass percentage concentration of the ethanol solution is 70-90%, the mass percentage concentration of the hot NaOH solution is 10-15%, the temperature is 40-60 ℃, the power of the ultrasonic cleaning is 800-1200W, the aluminum content in the high-purity aluminum block is more than 99%, and the copper content in the high-purity copper block is more than 99%.
As a further improvement of the invention, the temperature of the hot-dip assistant in the step S3 is 40-50 ℃.
As a further improvement of the invention, in the step S4, the volume fraction of the nitrogen in the high-purity nitrogen is more than 99.995%, the introducing rate of the high-purity nitrogen is 2-5L/min, and the set temperature is 1200 ℃ and 1400 ℃.
As a further improvement of the invention, the organic silicon sealant is selected from one or a mixture of several of acetic acid type, ketoxime type, alcohol type, amide type, hydroxylamine type and ketone type organic silicon sealant.
As a further improvement of the invention, the nickel electroplating solution is prepared by the following raw materials in quantity: NiSO4·6H2O 500-600g/L，NaCl 10-20g/L，H3BO320-30g/L, 15-30mL/L of softening agent BSI, 2-801 mL/L of wetting agent MA, and 1.2mL/L of stabilizing agent PVA-1240.5.
As a further improvement of the invention, the electroplating process comprises the following steps: adopting 267mL of Hehr bath, collecting 250mL of plating solution, anode being 100mm × 60mm × 3mm pure nickel plate, cathode being 100mm × 65mm × 0.3mm brass sheet, temperature being 50-60 deg.C, pH being 3.5-4.5, cathode current density being 2-15A/dm2And the current is 2A, a glass rod is adopted to stir back and forth in parallel with the cathode near the cathode, the moving speed is 1 time/s, and the time is 5-10 min.
The invention further protects a metallized ceramic prepared by the method.
The invention further protects the use of the above described metallized ceramic in a magnetron.
The invention has the following beneficial effects: in the invention, because the temperature of the hot dip aluminum and copper alloy plating solution is high, aluminum is easy to generate aluminum oxide films, a plating assistant agent NH is used4Cl, and introduction of fluoride K2ZrF6NaF, which can form a continuous and complete protective film without pores on the surface of the white porcelain; simultaneously, the aluminum and copper alloy liquid can be immediately removed from the surface of the white porcelain when being immersed; the method has the advantages that the method has an adsorption and melting effect on some oxides, does not pollute the molten aluminum, and can improve the surface performance of the white porcelain by adding rare earth metal chlorides such as cerium chloride and lanthanum chloride, so that the grains are refined, and the addition of the cerium chloride and the lanthanum chloride has a synergistic effect;
according to the invention, a reasonable matching technology of hot-dip aluminum-copper alloy and ceramic crystalline phase particles is adopted, so that a metalized aluminum-copper alloy layer can be tightly combined with a ceramic body during sintering on the premise of not increasing the sintering temperature, and then a metalized nickel layer is plated on the metalized aluminum-copper alloy layer, so that the surface quality and tensile strength of a ceramic metalized layer are greatly improved, and the metal layer is uniform and fine;
the preparation method is simple in preparation process, the coverage rate is high when the aluminum-copper alloy is hot-dipped, the antenna can be reduced to 0 degree, perfect wetting is achieved, and the phenomenon of 'abnormal wetting' between the aluminum-copper alloy liquid and the surface of the annular ceramic matrix is generated; further, a metal nickel layer is electroplated on the surface of the alloy layer, so that the wall thickness of the ceramic metal layer is effectively increased, the phenomenon that the ceramic wall is broken down or cracked due to overlarge current generated by a magnetic field in the magnetron is avoided, and the service life of the magnetron is prolonged.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a scanning electron microscope image of the cross-sectional profile of a sample of hot-dip aluminized or copper on the surface of an annular ceramic substrate in example 3 of the present invention;
FIG. 2 is a transmission electron microscope image of the structure of the Al layer, the Cu layer and the Ni layer in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
S1, preparing the plating assistant agent:
the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)4Cl 70 parts, NaF 0.5 parts, K2ZrF670 parts of cerium chloride, 0.01 part of lanthanum chloride and 300 parts of water, and uniformly mixing the raw materials in proportion for later use;
s2, processing the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the grease on the surface by using 70wt% ethanol solution, wherein the ultrasonic cleaning power is 800W, then removing an oxide film on the surface by using 10wt% NaOH solution at 40 ℃, finally cleaning by using deionized water, and then putting into an oven for drying; the aluminum content in the high-purity aluminum block is more than 99%, and the copper content in the high-purity copper block is more than 99%;
s3, pretreatment: soaking the annular ceramic matrix in a plating assistant agent at 40 ℃ for 10min, and taking out for later use;
s4, hot-dip aluminum plating, copper alloy: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by hydroxylamine type organosilicon sealant, heating to 1200 ℃ after the sealant is dried, simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at a rate of 2L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing out the annular ceramic substrate together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling, and thus obtaining a uniform aluminum-copper alloy film with the thickness of 3-10 micrometers on the ceramic surface;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; placing the end face of the ring-shaped ceramic substrate which is metallized upwards into a graphite guide rail, placing the high-purity aluminum block and the high-purity copper block which are cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat the furnace body until the temperature is 1200 ℃ after the sealant is dried, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 2L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the ring-shaped ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the ring-shaped ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the ring-shaped ceramic substrate out at a constant speed together with the aluminum-copper alloy liquid attached to the surface and gradually cooling the ring-shaped ceramic substrate;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum copper alloy films of the inner side wall and the outer side wall by using an electric-shock method, and then putting the aluminum copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece, wherein the ultrasonic cleaning power is 100W;
s7, nickel layer electroplating: soaking the metallized ceramic piece obtained in the step S6 in nickel electroplating solution for electroplating;
the electroplating solution is prepared from the following raw materials in parts by weight: NiSO4·6H2O 500g/L，NaCl 10g/L，H3BO320g/L, 15mL/L of softening agent BSI, 801 mL/L of wetting agent MA, 1240.5 mL/L of stabilizing agent PVA, and the balance of deionized water;
the electroplating process comprises the following steps: using 267mL of Hell cell, 250mL of plating solution was taken, the anode was a pure nickel plate of 100mm × 60mm × 3mm, and the cathode was a pure nickel plate of 100mm × 65mm × 0.3mmBrass sheet, temperature 50 deg.C, pH 3.5, cathode current density 2A/dm2And the current is 2A, a glass rod is adopted to stir back and forth in parallel with the cathode near the cathode, the moving speed is 1 time/s, and the time is 5 min.
S8, cleaning the side wall again: mechanically polishing the inner side wall and the outer side wall of the metalized ceramic piece electroplated in the step S7 again, wherein the surface roughness Ra is 0.1 micrometer; and then putting the ceramic ring into deionized water for ultrasonic cleaning for 10min to obtain the microwave magnetron insulating ceramic ring.
Example 2
S1, preparing the plating assistant agent:
the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)4120 parts of Cl, 1.5 parts of NaF and K2ZrF6120 parts of cerium chloride, 0.1 part of lanthanum chloride and 500 parts of water, and the raw materials are uniformly mixed according to a proportion for later use;
s2, processing the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the surface of the high-purity aluminum block and the high-purity copper block by using a 90wt% ethanol solution, wherein the ultrasonic cleaning power is 1200W, removing an oxide film on the surface of the high-purity aluminum block and the high-purity copper block by using a 15wt% NaOH solution at 60 ℃, cleaning the high-purity aluminum block and the high-purity copper block by using deionized water, and drying the high-purity; the aluminum content in the high-purity aluminum block is more than 99%, and the copper content in the high-purity copper block is more than 99%;
s3, pretreatment: soaking the annular ceramic matrix in plating assistant agent at 40-50 deg.C for 20min, and taking out;
s4, hot-dip aluminum plating, copper alloy: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an alcohol type organic silicon sealant, heating to 1400 ℃ after the sealant is dried, simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate with the aluminum-copper alloy liquid attached to the surface at the constant speed and gradually cooling, so that a uniform aluminum-copper alloy film with the thickness of 3-10 micrometers can be obtained on the surface of the ceramic;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; placing the metalized end face of the annular ceramic substrate upwards into a graphite guide rail, placing the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat the furnace body to 1400 ℃ after the sealant is dried, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at a rate of 5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate out at a constant speed together with the aluminum-copper alloy liquid attached to the surface and gradually cooling the annular ceramic substrate, so that a uniform aluminum-copper alloy film with the thickness of 3-10 micrometers can;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum copper alloy films of the inner side wall and the outer side wall by using an electric-shock method, and then putting the aluminum copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece, wherein the ultrasonic cleaning power is 150W;
s7, nickel layer electroplating: soaking the metallized ceramic piece obtained in the step S6 in nickel electroplating solution for electroplating;
the electroplating solution is prepared from the following raw materials in parts by weight: NiSO4·6H2O 600g/L，NaCl 20g/L，H3BO330g/L, 30mL/L of softening agent BSI, 30mL/L of wetting agent MA-802 mL/L, stabilizer PVA-1241.2 mL/L and the balance of deionized water;
the electroplating process comprises the following steps: taking 250mL of plating solution by adopting a 267mL hall bath, taking a pure nickel plate with an anode of 100mm multiplied by 60mm multiplied by 3mm and a brass sheet with a cathode of 100mm multiplied by 65mm multiplied by 0.3mm, controlling the temperature at 60 ℃, the pH value at 4.5 and the cathode current density at 15A/dm2And the current is 2A, a glass rod is adopted to stir back and forth in parallel with the cathode near the cathode, the moving speed is 1 time/s, and the time is 10 min.
S8, cleaning the side wall again: mechanically polishing the inner side wall and the outer side wall of the metalized ceramic piece electroplated in the step S7 again, wherein the surface roughness Ra is 0.3 micrometer; and then putting the ceramic ring into deionized water for ultrasonic cleaning for 15min to obtain the microwave magnetron insulating ceramic ring.
Example 3
S1, preparing the plating assistant agent:
the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)4Cl 100 parts, NaF 1 part and K2ZrF6100 parts of cerium chloride, 0.05 part of lanthanum chloride and 400 parts of water, and uniformly mixing the raw materials in proportion for later use;
s2, processing the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the surface of the aluminum block and the high-purity copper block by using 80wt% ethanol solution, wherein the ultrasonic cleaning power is 1000W, removing an oxide film on the surface of the aluminum block and the high-purity copper block by using 12wt% NaOH solution at 50 ℃, finally cleaning the aluminum block and the high-purity copper block by using deionized water, and then putting the aluminum block and the high-purity copper block into an oven; the aluminum content in the high-purity aluminum block is more than 99%, and the copper content in the high-purity copper block is more than 99%;
s3, pretreatment: soaking the annular ceramic matrix in a plating assistant agent at 45 ℃ for 15min, and taking out for later use;
s4, hot-dip aluminum plating, copper alloy: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an acetic acid type organic silicon sealant, after the sealant is dried, starting to heat the annular ceramic substrate to 1300 ℃, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate out together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a layer of uniform aluminum-copper alloy film with the thickness of 3-;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; placing the metalized end face of the annular ceramic substrate upwards into a graphite guide rail, placing the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat the furnace body until 1300 ℃ after the sealant is dried, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a uniform aluminum-copper alloy film with the thickness of 3-10 micrometers can be;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum copper alloy films of the inner side wall and the outer side wall by means of current and low temperature, and then putting the aluminum copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece, wherein the ultrasonic cleaning power is 120W;
s7, nickel layer electroplating: soaking the metallized ceramic piece obtained in the step S6 in nickel electroplating solution for electroplating;
the electroplating solution is prepared from the following raw materials in parts by weight: NiSO4·6H2O 550g/L，NaCl 15g/L，H3BO325g/L, 22mL/L of softening agent BSI, 801.5 mL/L of wetting agent MA, 1240.7 mL/L of stabilizing agent PVA, and the balance of deionized water;
the electroplating process comprises the following steps: taking 250mL of plating solution by adopting a 267mL hall bath, taking a pure nickel plate with an anode of 100mm multiplied by 60mm multiplied by 3mm and a brass sheet with a cathode of 100mm multiplied by 65mm multiplied by 0.3mm, controlling the temperature to be 55 ℃, the pH value to be 4 and the cathode current density to be 8A/dm2And the current is 2A, a glass rod is adopted to stir back and forth in parallel with the cathode near the cathode, the moving speed is 1 time/s, and the time is 7 min.
S8, cleaning the side wall again: mechanically polishing the inner side wall and the outer side wall of the metalized ceramic piece electroplated in the step S7 again, wherein the surface roughness Ra is 0.2 micrometer; and then putting the ceramic ring into deionized water for ultrasonic cleaning for 12min to obtain the microwave magnetron insulating ceramic ring.
The surface and profile of the hot dip aluminized and copper samples of the toroidal ceramic substrate surface were observed using a scanning electron microscope model SSX-550 from shimadzu corporation, japan, as shown in fig. 1. The hot dip aluminum and copper plating process of the annular ceramic matrix can obtain uniform and flat aluminum and copper film layers on the surface of the annular ceramic matrix, and as can be seen from the figure, the interface between the annular ceramic matrix and the aluminum and copper film layers is tightly connected without holes and cracks, so that the hot dip aluminum and copper plating process can form uniform aluminum and copper films on the annular ceramic matrix, and the phenomenon of 'super-wetting' of the aluminum, the copper and the annular ceramic matrix occurs.
The structure of the Al, Cu and Ni layers was observed by JEOL-2011 transmission electron microscope, and the result is shown in FIG. 2, which shows that the step-like protrusions at the interface of the Al, Cu and Ni layers have a height of about 3-4 nm and a very flat surface. And from the crystal lattice image, the steps are obviously formed by epitaxial growth on the surface of the aluminum and copper film layers. Therefore, the formed metal layer is uniform and fine.
Comparative example 1
Compared with the plating assistant agent of the embodiment 3, lanthanum chloride is not added in the plating assistant agent, and other conditions are not changed.
S1, preparing the plating assistant agent:
the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)4Cl 100 parts, NaF 1 part and K2ZrF6100 parts of cerium chloride and 400 parts of water, and uniformly mixing the raw materials in proportion for later use;
s2, processing the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the surface of the aluminum block and the high-purity copper block by using 80wt% ethanol solution, wherein the ultrasonic cleaning power is 1000W, removing an oxide film on the surface of the aluminum block and the high-purity copper block by using 12wt% NaOH solution at 50 ℃, finally cleaning the aluminum block and the high-purity copper block by using deionized water, and then putting the aluminum block and the high-purity copper block into an oven; the aluminum content in the high-purity aluminum block is more than 99%, and the copper content in the high-purity copper block is more than 99%;
s3, pretreatment: soaking the annular ceramic matrix in a plating assistant agent at 45 ℃ for 15min, and taking out for later use;
s4, hot-dip aluminum plating, copper alloy: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an acetic acid type organic silicon sealant, after the sealant is dried, starting to heat the annular ceramic substrate to 1300 ℃, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate out together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a layer of uniform aluminum-copper alloy film with the thickness of 3-;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; placing the metalized end face of the annular ceramic substrate upwards into a graphite guide rail, placing the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat the furnace body until 1300 ℃ after the sealant is dried, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a uniform aluminum-copper alloy film with the thickness of 3-10 micrometers can be;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum copper alloy films of the inner side wall and the outer side wall by means of current and low temperature, and then putting the aluminum copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece, wherein the ultrasonic cleaning power is 120W;
s7, nickel layer electroplating: soaking the metallized ceramic piece obtained in the step S6 in nickel electroplating solution for electroplating;
the electroplating solution is prepared from the following raw materials in parts by weight: NiSO4·6H2O 550g/L，NaCl 15g/L，H3BO325g/L, 22mL/L of softening agent BSI, 801.5 mL/L of wetting agent MA, 1240.7 mL/L of stabilizing agent PVA, and the balance of deionized water;
electroplating ofThe process comprises the following steps: taking 250mL of plating solution by adopting a 267mL hall bath, taking a pure nickel plate with an anode of 100mm multiplied by 60mm multiplied by 3mm and a brass sheet with a cathode of 100mm multiplied by 65mm multiplied by 0.3mm, controlling the temperature to be 55 ℃, the pH value to be 4 and the cathode current density to be 8A/dm2And the current is 2A, a glass rod is adopted to stir back and forth in parallel with the cathode near the cathode, the moving speed is 1 time/s, and the time is 7 min.
S8, cleaning the side wall again: mechanically polishing the inner side wall and the outer side wall of the metalized ceramic piece electroplated in the step S7 again, wherein the surface roughness Ra is 0.2 micrometer; and then putting the ceramic ring into deionized water for ultrasonic cleaning for 12min to obtain the microwave magnetron insulating ceramic ring.
Comparative example 2
Compared with the example 3, cerium chloride is not added into the plating assistant agent, and other conditions are not changed.
S1, preparing the plating assistant agent:
the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)4Cl 100 parts, NaF 1 part and K2ZrF6100 parts of lanthanum chloride, 0.05 part of lanthanum chloride and 400 parts of water, and uniformly mixing the raw materials in proportion for later use;
s2, processing the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the surface of the aluminum block and the high-purity copper block by using 80wt% ethanol solution, wherein the ultrasonic cleaning power is 1000W, removing an oxide film on the surface of the aluminum block and the high-purity copper block by using 12wt% NaOH solution at 50 ℃, finally cleaning the aluminum block and the high-purity copper block by using deionized water, and then putting the aluminum block and the high-purity copper block into an oven; the aluminum content in the high-purity aluminum block is more than 99%, and the copper content in the high-purity copper block is more than 99%;
s3, pretreatment: soaking the annular ceramic matrix in a plating assistant agent at 45 ℃ for 15min, and taking out for later use;
s4, hot-dip aluminum plating, copper alloy: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an acetic acid type organic silicon sealant, after the sealant is dried, starting to heat the annular ceramic substrate to 1300 ℃, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate out together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a layer of uniform aluminum-copper alloy film with the thickness of 3-;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; placing the metalized end face of the annular ceramic substrate upwards into a graphite guide rail, placing the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat the furnace body until 1300 ℃ after the sealant is dried, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a uniform aluminum-copper alloy film with the thickness of 3-10 micrometers can be;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum copper alloy films of the inner side wall and the outer side wall by means of current and low temperature, and then putting the aluminum copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece, wherein the ultrasonic cleaning power is 120W;
s7, nickel layer electroplating: soaking the metallized ceramic piece obtained in the step S6 in nickel electroplating solution for electroplating;
the electroplating solution is prepared from the following raw materials in parts by weight: NiSO4·6H2O 550g/L，NaCl 15g/L，H3BO325g/L, 22mL/L of softening agent BSI, 801.5 mL/L of wetting agent MA, 1240.7 mL/L of stabilizing agent PVA, and the balance of deionized water;
the electroplating process comprises the following steps: taking 250mL of plating solution by adopting a 267mL hall bath, taking a pure nickel plate with an anode of 100mm multiplied by 60mm multiplied by 3mm and a brass sheet with a cathode of 100mm multiplied by 65mm multiplied by 0.3mm, controlling the temperature to be 55 ℃, the pH value to be 4 and the cathode current density to be 8A/dm2Current 2A, usingThe glass rod is reciprocally stirred in parallel with the cathode near the cathode, the moving speed is 1 time/s, and the time is 7 min.
S8, cleaning the side wall again: mechanically polishing the inner side wall and the outer side wall of the metalized ceramic piece electroplated in the step S7 again, wherein the surface roughness Ra is 0.2 micrometer; and then putting the ceramic ring into deionized water for ultrasonic cleaning for 12min to obtain the microwave magnetron insulating ceramic ring.
Comparative example 3
In contrast to example 3, the ring-shaped ceramic substrate was not subjected to the nickel electroplating process.
S1, preparing the plating assistant agent:
the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)4Cl 100 parts, NaF 1 part and K2ZrF6100 parts of cerium chloride, 0.05 part of lanthanum chloride and 400 parts of water, and uniformly mixing the raw materials in proportion for later use;
s2, processing the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the surface of the aluminum block and the high-purity copper block by using 80wt% ethanol solution, wherein the ultrasonic cleaning power is 1000W, removing an oxide film on the surface of the aluminum block and the high-purity copper block by using 12wt% NaOH solution at 50 ℃, finally cleaning the aluminum block and the high-purity copper block by using deionized water, and then putting the aluminum block and the high-purity copper block into an oven; the aluminum content in the high-purity aluminum block is more than 99%, and the copper content in the high-purity copper block is more than 99%;
s3, pretreatment: soaking the annular ceramic matrix in a plating assistant agent at 45 ℃ for 15min, and taking out for later use;
s4, hot-dip aluminum plating, copper alloy: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an acetic acid type organic silicon sealant, after the sealant is dried, starting to heat the annular ceramic substrate to 1300 ℃, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate out together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a layer of uniform aluminum-copper alloy film with the thickness of 3-;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; placing the metalized end face of the annular ceramic substrate upwards into a graphite guide rail, placing the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat the furnace body until 1300 ℃ after the sealant is dried, and simultaneously introducing high-purity nitrogen (the volume fraction of the nitrogen is more than 99.995%) at the rate of 3.5L/min, after the aluminum and the copper in the graphite crucible are melted, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate together with the aluminum-copper alloy liquid attached to the surface at a constant speed and gradually cooling the annular ceramic substrate, so that a uniform aluminum-copper alloy film with the thickness of 3-10 micrometers can be;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum copper alloy films of the inner side wall and the outer side wall by means of current and low temperature, and then putting the aluminum copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece, wherein the ultrasonic cleaning power is 120W;
test example 1
The metallized ceramics prepared in examples 1-3 of the present invention and comparative examples 1-3 were subjected to performance tests, and the results are shown in table 1.
TABLE 1
| Group of | Metal film layer (mum) | Tensile strength (MPa) | Service life of magnetron (year) | Corrosion resistance | Temperature tolerance (. degree.C.) |
| Example 1 | 17 | 17.5 | 10 | Good effect | 1000 |
| Example 2 | 19 | 17.4 | 10 | Good effect | 1050 |
| Example 3 | 22 | 17.9 | 10 | Good effect | 1070 |
| Comparative example 1 | 14 | 10.2 | 7 | In general | 670 |
| Comparative example 2 | 15 | 12.3 | 7 | In general | 700 |
| Comparative example 3 | 7 | 13.5 | 4 | Is poor | 720 |
As can be seen from the above table, the metallized ceramic prepared by the method of the invention has good tensile strength, obviously prolongs the service life after being made into a magnetron, and has good corrosion resistance and heat resistance.
Lanthanum chloride and cerium chloride are not added in the comparative example 1 and the comparative example 2 respectively, so that the surface performance of the white porcelain is reduced, the structure is loose when an aluminum-copper film layer is formed, tight connection cannot be realized, and the performance of the obtained metalized ceramic is reduced;
comparative example 3 adopts a hot-dip aluminum-copper alloy plating layer, only a single metal layer is provided, and the metal film is thin, so that the service life of the manufactured magnetron is greatly reduced, and the corrosion resistance and the heat resistance are poor.
Compared with the prior art, the invention uses the plating assistant agent NH because the hot-dip aluminum and copper alloy plating liquid has higher temperature and aluminum is easy to generate aluminum oxide films4Cl, and introduction of fluoride K2ZrF6NaF, which can form a continuous and complete protective film without pores on the surface of the white porcelain (annular ceramic matrix); simultaneously, the aluminum and copper alloy liquid can be immediately removed from the surface of the white porcelain (annular ceramic matrix) during immersion; the method has the advantages that the method has an adsorption and melting effect on some oxides, does not pollute the molten aluminum, and can improve the surface performance of the white porcelain (annular ceramic matrix) by refining grains by adding rare earth metal chlorides such as cerium chloride and lanthanum chloride, and the addition of the cerium chloride and the lanthanum chloride has a synergistic effect;
according to the invention, a reasonable matching technology of hot-dip aluminum-copper alloy and ceramic crystalline phase particles is adopted, so that a metalized aluminum-copper alloy layer can be tightly combined with a ceramic body during sintering on the premise of not increasing the sintering temperature, and then a metalized nickel layer is plated on the metalized aluminum-copper alloy layer, so that the surface quality and tensile strength of a ceramic metalized layer are greatly improved, and the metal layer is uniform and fine;
the preparation method is simple in preparation process, the coverage rate is high when the aluminum-copper alloy is hot-dipped, the antenna can be reduced to 0 degree, perfect wetting is achieved, and the phenomenon of 'abnormal wetting' between the aluminum-copper alloy liquid and the surface of the annular ceramic matrix is generated; further, a metal nickel layer is electroplated on the surface of the alloy layer, so that the wall thickness of the ceramic metal layer is effectively increased, the phenomenon that the ceramic wall is broken down or cracked due to overlarge current generated by a magnetic field in the magnetron is avoided, and the service life of the magnetron is prolonged.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A microwave magnetron insulating ceramic ring is characterized in that: the metal plating structure comprises an annular ceramic matrix and metallization layers at two ends of the annular ceramic matrix; the processing method of the metallization layer comprises the following steps:
s1, preparing a plating assistant agent: the plating assistant agent comprises NH4Cl、NaF、K2ZrF6Cerium chloride, lanthanum chloride and water, and the raw materials are uniformly mixed according to a proportion for later use;
the plating assistant agent is prepared from the following raw materials in parts by weight: NH (NH)470-120 parts of Cl, 0.5-1.5 parts of NaF and K2ZrF670-120 parts of cerium chloride, 0.01-0.1 part of lanthanum chloride and 500 parts of water 300-;
s2, treating the high-purity aluminum block and the high-purity copper block: respectively putting a high-purity aluminum block and a high-purity copper block into an ultrasonic generator, ultrasonically cleaning the grease on the surface by using an ethanol solution, removing an oxide film on the surface by using a hot NaOH solution, finally cleaning by using deionized water, and then putting into an oven for drying;
s3, pretreatment: soaking the annular ceramic matrix in the hot plating assistant for 10-20min, and taking out for later use;
s4, single-side hot-dip aluminum plating and copper alloy plating: putting the annular ceramic substrate processed in the step S3 into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block cleaned in the step S2 into a graphite crucible, sealing the furnace body by using an organic silicon sealant, starting to heat the furnace body until the temperature is set after the sealant is dried, simultaneously introducing high-purity nitrogen with a certain flow rate, pushing the annular ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed after the aluminum and the copper in the graphite crucible are melted, contacting the annular ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the annular ceramic substrate out at a constant speed together with the aluminum-copper alloy liquid attached to the surface, and gradually cooling the annular ceramic substrate to obtain single-sided metalized layer, wherein the metalized layer is a uniform aluminum-copper alloy film with the thickness of 3-10 microns;
s5, double-sided hot-dip aluminum plating and copper alloy plating: carrying out double-sided metallization on the single-sided metalized annular ceramic obtained in the step S4; putting the end face of the ring-shaped ceramic substrate which is metalized upwards into a graphite guide rail, putting the high-purity aluminum block and the high-purity copper block which are cleaned in the step S2 into a graphite crucible, sealing a furnace body by using an organic silicon sealant, starting to heat until the set temperature is reached after the sealant is dried, simultaneously introducing high-purity nitrogen with a certain flow rate, pushing the ring-shaped ceramic substrate into the guide rail from an inlet below the guide rail at a constant speed after the aluminum and the copper in the graphite crucible are melted, contacting the ring-shaped ceramic substrate with molten aluminum-copper alloy liquid through a window of the graphite guide rail, then pushing the ring-shaped ceramic substrate out together with the aluminum-copper alloy liquid attached to the surface and gradually cooling to obtain double-sided metalized ring-shaped ceramic, wherein the metalized layer is a uniform aluminum-copper alloy film with the thickness of 3;
s6, side wall cleaning: mechanically polishing the inner side wall and the outer side wall of the double-sided metalized annular ceramic obtained in the step S5, polishing off aluminum-copper alloy films of the inner side wall and the outer side wall by using an electric-shock method, and then putting the aluminum-copper alloy films into water for ultrasonic cleaning for 10-15min to obtain a metalized ceramic piece;
s7, nickel layer electroplating: soaking the metallized ceramic piece obtained in the step S6 in nickel electroplating solution for electroplating;
s8, cleaning the side wall again: mechanically polishing the inner side wall and the outer side wall of the metalized ceramic piece electroplated in the step S7 again, wherein the surface roughness Ra is 0.1-0.3 micrometer; and then putting the ceramic ring into deionized water for ultrasonic cleaning for 10-15min to obtain the microwave magnetron insulating ceramic ring.
2. The microwave magnetron insulating ceramic ring as claimed in claim 1, wherein the concentration of the ethanol solution in step S2 is 70-90% by mass, the concentration of the hot NaOH solution in mass is 10-15% by mass, the temperature is 40-60 ℃, the power of the ultrasonic cleaning is 800-1200W, the content of aluminum in the high-purity aluminum block is greater than 99%, and the content of copper in the high-purity copper block is greater than 99%.
3. The microwave magnetron insulating ceramic ring according to claim 1, wherein the temperature of the thermal promoter in step S3 is 40-50 ℃.
4. The microwave magnetron insulating ceramic ring as claimed in claim 1, wherein the volume fraction of nitrogen in the high purity nitrogen gas in step S4 is greater than 99.995%, the flow rate of the high purity nitrogen gas is 2-5L/min, and the set temperature is 1200-1400 ℃.
5. The microwave magnetron insulating ceramic ring according to claim 1, wherein the silicone sealant is one or a mixture of several of acetic acid type, ketoxime type, alcohol type, amide type, hydroxylamine type and ketone type silicone sealants.
6. The microwave magnetron insulating ceramic ring according to claim 1, wherein the nickel plating solution is prepared quantitatively from the following raw materials: NiSO4·6H2O 500-600g/L，NaCl 10-20g/L，H3BO320-30g/L, softening agent BSI15-30mL/L, wetting agent MA-801-2mL/L and stabilizer PVA-1240.5-1.2 mL/L.
7. The microwave according to claim 1The magnetron insulating ceramic ring is characterized in that the electroplating process comprises the following steps: adopting 267mL of Hehr bath, collecting 250mL of plating solution, anode being 100mm × 60mm × 3mm pure nickel plate, cathode being 100mm × 65mm × 0.3mm brass sheet, temperature being 50-60 deg.C, pH being 3.5-4.5, cathode current density being 2-15A/dm2And the current is 2A, a glass rod is adopted to stir back and forth in parallel with the cathode near the cathode, the moving speed is 1 time/s, and the time is 5-10 min.
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Denomination of invention: Microwave magnetron insulating ceramic ring Effective date of registration: 20210722 Granted publication date: 20201023 Pledgee: Loudi Xinglou financing Company limited by guarantee Pledgor: HUNAN MEICHENG CERAMIC TECHNOLOGY Co.,Ltd. Registration number: Y2021430000032 |