CN103498157A - Method for preparing silvered layer on 4J34 fe-ni-co ceramic sealing alloy - Google Patents
Method for preparing silvered layer on 4J34 fe-ni-co ceramic sealing alloy Download PDFInfo
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- CN103498157A CN103498157A CN201310476553.XA CN201310476553A CN103498157A CN 103498157 A CN103498157 A CN 103498157A CN 201310476553 A CN201310476553 A CN 201310476553A CN 103498157 A CN103498157 A CN 103498157A
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Abstract
The invention relates to a method for preparing a silvered layer on a 4J34 fe-ni-co ceramic sealing alloy. By immersing a matrix in a 200-250g/L of NiCl26H20 and 180-220g/L of HCi (30%) solution for electrifying and nickeling, nickel and cobalt are quite similar in property, unstable in air and extremely easy to oxidize to form an oxidation film difficult to remove, so that bonding force between a plating and the matrix is effected. Consequently, the oxidation film on the surface of a part needs to be removed in an electroplating process, and the surface of the matrix needs to be fully activated. At normal temperature, a certain amount of hydrochloric acid contained in a nickeling solution has strong chemical dissolving effect on a metal oxide of the steel part and is slow in dissolving of the matrix, so that metal of the matrix can be fully exposed by selecting a hydrochloric acid weak corrosive solution proper in concentrate. By adjusting nickel chloride nickeling processing before nickeling of the 4J34 fe-ni-co ceramic sealing alloy and adopting a pre-nickeling solution formed by nickel chlorid and hydrochloric acid, the surface of the part can be fully activated in the process of electroplating, and the bonding force of a nickel layer and the matrix is improved.
Description
Technical field
The invention belongs to the preparing technical field of silvered film, be specifically related to a kind of method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy.
Background technology
Xxx-25 semiconductor discharge plug housing, material is the 4J34 fe-Ni-Co ceramic sealing alloy, surface needs silver-plated processing.In triturating, still deposit housing and binding force of cladding material is poor through technological test repeatedly, bubbling appears in coating, obscission.Due to the work under bad environment of xxx-25 semiconductor discharge plug housing, meet the housing coating of working and not come off under-55～800 ℃ of conditions, technology difficulty is very large, and plating our factory and the same industry of 4J34 fe-Ni-Co ceramic sealing alloy material also have no and introduced.Therefore in order to meet the development needs of xxx engine igniting system, existing processing method has been proposed to challenge.
Due to the 4J34 fe-Ni-Co ceramic sealing alloy, nickeliferous 28.5～29.5%, cobalt 19.5～20.5%, all the other are iron; Very similar with cobalt character because of nickel, unstable in air, very easily oxidation, form the oxide film of the more difficult removal of one deck, thereby affect the bonding force between coating and matrix.Meet the 4J34 fe-Ni-Co ceramic sealing alloy housing coating of working and do not come off under-55～800 ℃ of conditions, technology difficulty is very large, and plating our factory and the same industry of 4J34 fe-Ni-Co ceramic sealing alloy material also have no and introduced.
Obviously, current processing method can not meet the silver-plated requirement of aeronautical product part of new generation.
Summary of the invention
For fear of the deficiencies in the prior art part, the present invention proposes a kind of method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy.
A kind of method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy is characterized in that step is as follows:
Step 1: adopt organic solution to clean and prepare silver-plated matrix surface, then carry out electrochemical degreasing; Adopt again higher than after the flowing water flushing of 50 ℃, adopting again the room temperature flowing water to rinse; Adopting HCL to be corroded rear employing room temperature flowing cool water rinses;
Step 2: the matrix after processing is submerged in electroplating solution to the nickel plating of being switched on, wherein the temperature of nickel plating solution is room temperature, in electroplating process, electrical current is 5-10A/dm2: from matrix submergence nickel plating solution constantly, electroplating time 3min～5min, then matrix is taken out from nickel plating solution, at room temperature adopt the deionized water rinsing matrix; Described electroplating solution is: the mixing solutions of the NiCl26H20 of 200-250g/L and the HCl of 180-220g/L (30%);
Step 3: the matrix after step 2 is processed is submerged in cyanide electroplating solution, and wherein the copper plating solution temperature is 30 ℃ ± 10 ℃, and Immersion time is 5min～10min; After matrix is taken out from copper plating solution, at room temperature use the deionized water rinsing matrix;
Step 4: the matrix after step 3 is processed is submerged in cyanide silver plating solution, and wherein the silver plating solution temperature is room temperature, and Immersion time is 30min～50min; After matrix is taken out from silver plating solution, then use the deionized water rinsing matrix under room temperature; After being dried up, matrix surface obtains silvered film at matrix surface.
It is 0.5min～3min that described step 2 adopts the flush time of deionized water rinsing matrix.
The deionization electrical conductivity of water that described step 2 adopts is not more than 0.5 μ S/cm.
It is 0.5min～3min that described step 3 adopts the flush time of deionized water rinsing matrix.
It is 0.5min～3min that described step 4 adopts the flush time of deionized water rinsing matrix.
Organic solution in described step 1 is aviation spirit.
The oil removing solution temperature of the electrochemical degreasing in described step 1 is 70 ℃, and the oil removing time is 0.1min, electric current 5-10A/dm2.
The effective component content except oil solution of the electrochemical degreasing in described step 1 is: the NaOH of 10g/L, the Na of 40g/L
3pO
4, the Na of 3g/L
2siO
4.
A kind of method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy that the present invention proposes, by matrix being submerged into to the NiCl26H20 of 200-250g/L, the nickel plating of being switched in the HCl of 180-220g/L (30%) solution, because of nickel very similar with cobalt character, unstable in air, very easily oxidation, form the oxide film of the more difficult removal of one deck, thereby affect the bonding force between coating and matrix.Therefore to remove the oxide film of piece surface on electroplating technology, fully activate matrix surface.Under normal temperature, contain a certain amount of hydrochloric acid in nickel plating solution the metal oxide of steel-iron components is had to stronger chemical dissolution effect, and comparatively slow to the dissolving of matrix, select the weak corrosive fluid of hydrochloric acid that concentration is suitable that matrix metal is fully come out.
The present invention, by adjusting the silver-plated front nickelous chloride Nickel Plating Treatment of 4J34 fe-Ni-Co ceramic sealing alloy, adopts nickelous chloride and hydrochloric acid to form pre-nickel plating solution, in electroplating process, can activate fully piece surface, improves the bonding force of nickel dam and matrix.
Embodiment
Now the invention will be further described in conjunction with the embodiments:
Embodiment 1:
The method for preparing silvered film at the 4J34 fe-Ni-Co ceramic sealing alloy in the present embodiment comprises the following steps:
Step 1: matrix is processed, and wherein basic material is the 4J34 fe-Ni-Co ceramic sealing alloy; The described method that matrix is processed comprises the following steps:
Step a: adopt organic solution to clean matrix surface, the organic solution adopted in the present embodiment is aviation spirit;
Step b: the matrix after cleaning is carried out to electrochemical degreasing; Except the oil solution effective ingredient, multiple choices can be arranged in the electrochemical deoiling process in prior art, the oil solution effective component content that removes in the present embodiment is: the NaOH of 10g/L, the Na of 40g/L
3pO
4, the Na of 3g/L
2siO
4; In the present embodiment, the oil removing solution temperature is 70 ℃, and the oil removing time is 0.1min, electric current 5-10A/dm2;
Step c: after adopting the flowing water flushing matrix 0.5min that temperature is 50 ℃, adopt again the room temperature flowing water to rinse matrix 1min;
Steps d: adopt the HCL of 300g/L to be corroded matrix, etching time is 3min;
Step e: the matrix after the deionized water rinsing corrosion under the employing room temperature, flush time is 0.5min;
Whole step 1 before the 4J34 fe-Ni-Co ceramic sealing alloy prepares silvered film, is processed matrix carrying out, and the present embodiment is also to have selected existing treatment process commonly used.
Step 2: the matrix that will obtain step 1 is submerged into the NiCl26H20 of 200g/L, the nickel plating of being switched in the HCl of 180g/L (30%) solution, wherein the temperature of nickel plating solution is room temperature, electrical current 5-10A/dm2 in electroplating process: from matrix submergence nickel plating solution constantly, electroplating time 3min～5min, then matrix is taken out from nickel plating solution, and adopt specific conductivity under room temperature to be not more than the deionized water rinsing matrix of 0.5 μ S/cm, flush time is 0.5min～3min;
Step 3: the matrix after step 2 is processed is submerged in cyanide electroplating solution, and wherein the copper plating solution temperature is 30 ℃ ± 10 ℃, and Immersion time is 5min～10min; After matrix is taken out from copper plating solution, with the deionized water rinsing matrix under room temperature, flush time is 0.5min～3min;
Step 4: the matrix after step 3 is processed is submerged in cyanide silver plating solution, and wherein the silver plating solution temperature is room temperature, and Immersion time is 30min～50min; After matrix is taken out from silver plating solution, with the deionized water rinsing matrix under room temperature, flush time is 0.5min～3min; After being dried up, matrix surface obtains silvered film at matrix surface.
Embodiment 2:
Step 1: matrix is processed, and wherein basic material is the 4J34 fe-Ni-Co ceramic sealing alloy; The described method that matrix is processed comprises the following steps:
Step a: adopt organic solution to clean matrix surface, the organic solution adopted in the present embodiment is aviation spirit;
Step b: the matrix after cleaning is carried out to electrochemical degreasing; Except the oil solution effective ingredient, multiple choices can be arranged in the electrochemical deoiling process in prior art, the oil solution effective component content that removes in the present embodiment is: the NaOH of 10g/L, the Na of 40g/L
3pO
4, the Na of 3g/L
2siO
4; In the present embodiment, the oil removing solution temperature is 70 ℃, and the oil removing time is 0.1min, electric current 5-10A/dm2;
Step c: after adopting the flowing water flushing matrix 0.5min that temperature is 50 ℃, adopt again the room temperature flowing water to rinse matrix 1min;
Steps d: adopt the HCL of 300g/L to be corroded matrix, etching time is 3min;
Step e: the matrix after the deionized water rinsing corrosion under the employing room temperature, flush time is 0.5min;
Whole step 1 before the 4J34 fe-Ni-Co ceramic sealing alloy prepares silvered film, is processed matrix carrying out, and the present embodiment is also to have selected existing treatment process commonly used.
Step 2: the matrix that will obtain step 1 is submerged into the NiCl26H20 of 250g/L, the nickel plating of being switched in the HCl of 220g/L (30%) solution, wherein the temperature of nickel plating solution is room temperature, electrical current 5-10A/dm2 in electroplating process: from matrix submergence nickel plating solution constantly, electroplating time 3min～5min, then matrix is taken out from nickel plating solution, and adopt specific conductivity under room temperature to be not more than the deionized water rinsing matrix of 0.5 μ S/cm, flush time is 0.5min～3min;
Step 3: the matrix after step 2 is processed is submerged in cyanide electroplating solution, and wherein the copper plating solution temperature is 30 ℃ ± 10 ℃, and Immersion time is 5min～10min; After matrix is taken out from copper plating solution, with the deionized water rinsing matrix under room temperature, flush time is 0.5min～3min;
Step 4: the matrix after step 3 is processed is submerged in cyanide silver plating solution, and wherein the silver plating solution temperature is room temperature, and Immersion time is 30min～50min; After matrix is taken out from silver plating solution, with the deionized water rinsing matrix under room temperature, flush time is 0.5min～3min; After being dried up, matrix surface obtains silvered film at matrix surface.
Embodiment 2:
Step 1: matrix is processed, and wherein basic material is the 4J34 fe-Ni-Co ceramic sealing alloy; The described method that matrix is processed comprises the following steps:
Step a: adopt organic solution to clean matrix surface, the organic solution adopted in the present embodiment is aviation spirit;
Step b: the matrix after cleaning is carried out to electrochemical degreasing; Except the oil solution effective ingredient, multiple choices can be arranged in the electrochemical deoiling process in prior art, the oil solution effective component content that removes in the present embodiment is: the NaOH of 10g/L, the Na of 40g/L
3pO
4, the Na of 3g/L
2siO
4; In the present embodiment, the oil removing solution temperature is 70 ℃, and the oil removing time is 0.1min, electric current 5-10A/dm2;
Step c: after adopting the flowing water flushing matrix 0.5min that temperature is 50 ℃, adopt again the room temperature flowing water to rinse matrix 1min;
Steps d: adopt the HCL of 300g/L to be corroded matrix, etching time is 3min;
Step e: the matrix after the deionized water rinsing corrosion under the employing room temperature, flush time is 0.5min;
Whole step 1 before the 4J34 fe-Ni-Co ceramic sealing alloy prepares silvered film, is processed matrix carrying out, and the present embodiment is also to have selected existing treatment process commonly used.
Step 2: the matrix that will obtain step 1 is submerged into the NiCl26H20 of 2300g/L, the nickel plating of being switched in the HCl of 200g/L (30%) solution, wherein the temperature of nickel plating solution is room temperature, electrical current 5-10A/dm2 in electroplating process: from matrix submergence nickel plating solution constantly, electroplating time 3min～5min, then matrix is taken out from nickel plating solution, and adopt specific conductivity under room temperature to be not more than the deionized water rinsing matrix of 0.5 μ S/cm, flush time is 0.5min～3min;
Step 3: the matrix after step 2 is processed is submerged in cyanide electroplating solution, and wherein the copper plating solution temperature is 30 ℃ ± 10 ℃, and Immersion time is 5min～10min; After matrix is taken out from copper plating solution, with the deionized water rinsing matrix under room temperature, flush time is 0.5min～3min;
Step 4: the matrix after step 3 is processed is submerged in cyanide silver plating solution, and wherein the silver plating solution temperature is room temperature, and Immersion time is 30min～50min; After matrix is taken out from silver plating solution, with the deionized water rinsing matrix under room temperature, flush time is 0.5min～3min; After being dried up, matrix surface obtains silvered film at matrix surface.
Step 2 is one of key technical features of the present invention, by matrix being submerged into to the NiCl26H20 of 200-250g/L, the nickel plating of being switched in the HCl of 180-220g/L (30%) solution, because of nickel very similar with cobalt character, unstable in air, very easily oxidation, form the oxide film of the more difficult removal of one deck, thereby affect the bonding force between coating and matrix.Therefore to remove the oxide film of piece surface on electroplating technology, fully activate matrix surface.Under normal temperature, contain a certain amount of hydrochloric acid in nickel plating solution the metal oxide of steel-iron components is had to stronger chemical dissolution effect, and comparatively slow to the dissolving of matrix, select the weak corrosive fluid of hydrochloric acid that concentration is suitable that matrix metal is fully come out.
The present embodiment obtains silvered film and has passed through 800 ℃ of tests of GJB150.3-86 high temperature test temperature, meets the technical requirement of aeronautical product part of new generation.
Claims (8)
1. a method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy is characterized in that step is as follows:
Step 1: adopt organic solution to clean and prepare silver-plated matrix surface, then carry out electrochemical degreasing; Adopt again higher than after the flowing water flushing of 50 ℃, adopting again the room temperature flowing water to rinse; Adopting HCL to be corroded rear employing room temperature flowing cool water rinses;
Step 2: the matrix after processing is submerged in electroplating solution to the nickel plating of being switched on, wherein the temperature of nickel plating solution is room temperature, in electroplating process, electrical current is 5-10A/dm2: from matrix submergence nickel plating solution constantly, electroplating time 3min～5min, then matrix is taken out from nickel plating solution, at room temperature adopt the deionized water rinsing matrix; Described electroplating solution is: the mixing solutions of the NiCl26H20 of 200-250g/L and the HCl of 180-220g/L (30%);
Step 3: the matrix after step 2 is processed is submerged in cyanide electroplating solution, and wherein the copper plating solution temperature is 30 ℃ ± 10 ℃, and Immersion time is 5min～10min; After matrix is taken out from copper plating solution, at room temperature use the deionized water rinsing matrix;
Step 4: the matrix after step 3 is processed is submerged in cyanide silver plating solution, and wherein the silver plating solution temperature is room temperature, and Immersion time is 30min～50min; After matrix is taken out from silver plating solution, then use the deionized water rinsing matrix under room temperature; After being dried up, matrix surface obtains silvered film at matrix surface.
2. the method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy according to claim 1 is characterized in that: it is 0.5min～3min that described step 2 adopts the flush time of deionized water rinsing matrix.
3. the method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy according to claim 1 and 2 is characterized in that: the deionization electrical conductivity of water that described step 2 adopts is not more than 0.5 μ S/cm.
4. the method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy according to claim 1 is characterized in that: it is 0.5min～3min that described step 3 adopts the flush time of deionized water rinsing matrix.
5. the method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy according to claim 1 is characterized in that: it is 0.5min～3min that described step 4 adopts the flush time of deionized water rinsing matrix.
6. the method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy according to claim 1, it is characterized in that: the organic solution in described step 1 is aviation spirit.
7. the method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy according to claim 1, it is characterized in that: the oil removing solution temperature of the electrochemical degreasing in described step 1 is 70 ℃, the oil removing time is 0.1min, electric current 5-10A/dm2.
8. according to the described method for preparing silvered film on the 4J34 fe-Ni-Co ceramic sealing alloy of claim 1 or 7, it is characterized in that: the effective component content except oil solution of the electrochemical degreasing in described step 1 is: the NaOH of 10g/L, the Na of 40g/L
3pO
4, the Na of 3g/L
2siO
4.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021109788A1 (en) * | 2019-12-03 | 2021-06-10 | 中兴通讯股份有限公司 | Method for surface metalization of ceramic dielectric filter, and product and use thereof |
| CN115805236A (en) * | 2023-02-09 | 2023-03-17 | 西安稀有金属材料研究院有限公司 | Process for preparing kovar alloy/AgCu alloy composite foil strip |
-
2013
- 2013-10-12 CN CN201310476553.XA patent/CN103498157A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 张强等: "1J50材料镀镍工艺研究", 《涂装与电镀》, no. 3, 30 June 2008 (2008-06-30), pages 39 - 41 * |
| 邓正平: "镍基高温合金镀银工艺", 《电镀与精饰》, vol. 23, no. 1, 31 January 2001 (2001-01-31), pages 25 - 26 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021109788A1 (en) * | 2019-12-03 | 2021-06-10 | 中兴通讯股份有限公司 | Method for surface metalization of ceramic dielectric filter, and product and use thereof |
| CN115805236A (en) * | 2023-02-09 | 2023-03-17 | 西安稀有金属材料研究院有限公司 | Process for preparing kovar alloy/AgCu alloy composite foil strip |
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Application publication date: 20140108 |