CN106435679B - A method of reducing ceramic electroless nickel layer blistering - Google Patents
A method of reducing ceramic electroless nickel layer blistering Download PDFInfo
- Publication number
- CN106435679B CN106435679B CN201610924611.4A CN201610924611A CN106435679B CN 106435679 B CN106435679 B CN 106435679B CN 201610924611 A CN201610924611 A CN 201610924611A CN 106435679 B CN106435679 B CN 106435679B
- Authority
- CN
- China
- Prior art keywords
- nickel
- ceramic
- ceramic part
- plating
- nickel layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The present invention provides a kind of methods for reducing ceramic electroless nickel layer blistering, the method includes surface treatment, plating, flushing, dehydration, drying, thickness measuring, post-processing and nickel process, increased thickness measuring, last handling process effectively strengthen the adhesive strength between surface of ceramic parts and nickel coating in prior art basis, reduce the blister formation of surface of ceramic parts nickel coating.The method of the ceramic electroless nickel layer blistering of reduction of the invention can be widely applied for the field of electroplating of ceramic part, the especially plating nickel on surface of ceramic base molybdenum matter porous membrane part.
Description
Technical field
The invention belongs to electrovacuum technology fields, and in particular to a kind of method for reducing ceramic electroless nickel layer blistering.
Background technique
In electron tube process for making, in order to by the performances such as the high intensity of ceramic material, high temperature resistant, corrosion-resistant
One is incorporated into plasticity, the good processability of metal material, it is often necessary to airtightly weld ceramic part with metal parts
It is connected together, but ceramics are often good insulating materials, usual solder cannot infiltrate it, thus can not achieve and metal
It is directly connected to.
At present solution there are several types of: first, liquid phase process, this technique refers in Ceramic and metal joining
When, with the presence of a certain amount of liquid phase between interface, to promote the contact and phase counterdiffusion between substance, ceramics is made to stick in one with metal
It rises.Second, gas phase process, this technique refer under given conditions (in such as vacuum by high energy beam or plasma Hong
Hit), so that metal is become steam or ion deposition in ceramic surface, and then realize the connection of ceramics with metal.Third, solid phase work
Skill, this technique refer to that ceramics and metal keep two kinds of interfaces tight under certain outer plus condition (such as high pressure, high temperature) in solid form
, there is not liquid phase and reaches air-tight connection in contiguity touching.
It is still with the Activated Molybdenum-Manganese in liquid phase process in current large-scale production electron tube product both at home and abroad
Based on method, i.e., it is firmly sintered one layer of porous metal film based on molybdenum in ceramic surface, and at one layer of its electroplating surface
Nickel layer is to improve the free-running property of solder.But the case where nickel coating is easy to appear attachment loosely during nickel, and coating blisters, it is right
The intensity and air-tightness of Ceramic and metal joining bring adverse effect." the thin molybdenum powder pair of " vacuum electronics technology " fourth phase in 2014
The influence and analysis of problems of a 95% aluminium oxide ceramics metallization quality " text is disclosed using reduction current density, is reduced
The methods of heating rate and replacement nickel sulfamic acid system are blistered to alleviate nickel coating, although these methods subtract to a certain extent
The quantity and probability of nickel coating blistering are delayed, but have extended electroplating time, reduced production efficiency, especially change electric plating body
After system in nickel coating the impurity such as easy residual sulphur, can not thoroughly efficiently solve nickel coating blistering the problem of.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of methods for reducing ceramic electroless nickel layer blistering.
The method of the ceramic electroless nickel layer blistering of reduction of the invention the following steps are included:
A. it is surface-treated
Surface of ceramic parts oxidation and pollution condition are estimated, the pickling in acid solution by ceramic part obtains ceramic part I；
B. it is electroplated
Ceramic part I is immersed into nickel plating in nickel bath, obtains ceramic part II；
C. it rinses
Ceramic part II is rinsed with deionized water at normal temperature, obtains ceramic part III；
D. it is dehydrated
Ceramic part III is dehydrated in dehydrated alcohol, obtains ceramic part IV；
E. it dries up
Ceramic part IV is dried up with compressed air, obtains ceramic part V；
F. thickness measuring
Using the nickel layer thickness of calibrator measurement ceramic part V, as nickel layer thickness h < 2mm, step b ~ f is repeated；When
When nickel layer thickness 2mm≤h≤10mm, ceramic part VI is obtained, continues subsequent step；As nickel layer thickness h > 10mm, stop work
Make；
G. it post-processes
Ceramic part VI is subjected to vacuum heat treatment in a vacuum furnace, obtains ceramic part VII；
H. nickel
Ceramic part VII is subjected to nickel processing in hydrogen furnace, obtains required product after nickel.
The acid solution of the step a is the hydrochloric acid that percent by volume is 30% ~ 50%.
The mass percent of the plating nickel electrolyte of the step b is water 57.8%, nickel sulfate 25%, sodium sulphate 8%, sulfuric acid
Magnesium 5%, sodium chloride 0.7% and boric acid 3.5%；Or the mass percent of plating nickel electrolyte is water 53.5%, nickel sulfate 27.5%, sulphur
Sour sodium 9%, magnesium sulfate 5.5%, sodium chloride 0.8% and boric acid 3.7%；Or the mass percent of plating nickel electrolyte is water 49.1%, sulphur
Sour nickel 30%, sodium sulphate 10%, magnesium sulfate 6%, sodium chloride 0.9% and boric acid 4%.
The process conditions of the step b nickel plating: the temperature for plating nickel electrolyte is 35 DEG C ~ 40 DEG C, plates the pH of nickel electrolyte
Value is 4.0 ~ 4.5, and current density is 0.8 A/dm2~1.0A/dm2, plating solution keeps flowing during nickel plating.
The process conditions of the step g vacuum heat treatment: heating rate≤20 DEG C/min, holding temperature be 750 DEG C ~
850 DEG C, vacuum degree≤10-4Pa cools down after heat preservation with furnace.
The process conditions of the step h nickelization processing: heating rate≤20 DEG C/min, nickel temperature are 900 DEG C ± 10
DEG C, 5 min -10min of nickel time cools down after heat preservation with furnace.
The method of the ceramic electroless nickel layer blistering of reduction of the invention has the advantage that
(1) qualification rate is high, by controlling thickness and the post-processing of nickel coating, can plate out adhesion-tight on ceramic part surface layer
Nickel coating, the blistering rate of nickel coating is reduced within 3%；
(2) easy to operate, post-processing is only increased in existing bath system and process flow, has not been changed existing production stream
Journey.
The method of the ceramic electroless nickel layer blistering of reduction of the invention can be widely applied for the field of electroplating of ceramic part, especially
It is the plating nickel on surface of ceramic base molybdenum matter porous membrane part, and the attachment that can reinforce between surface of ceramic parts and nickel coating is strong
Degree, is effectively reduced the blister formation of surface of ceramic parts nickel coating.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail.
Embodiment 1
Step 1, by the ceramic annulus of the attached molybdenum in the surface of 30mm, pickling 5 ~ 20 seconds in 30% ~ 50% hydrochloric acid solution；
Step 2, by ceramic annulus nickel plating, the process conditions of nickel plating: plate nickel electrolyte mass percent be water 57.8%,
Nickel sulfate 25%, sodium sulphate 8%, magnesium sulfate 5%, sodium chloride 0.7% and boric acid 3.5%, the temperature for plating nickel electrolyte is 35 DEG C ~ 40
DEG C, the pH value for plating nickel electrolyte is 4.0 ~ 4.5, and current density is 0.8 A/dm2~1.0A/dm2, plating solution keeps stream during nickel plating
It is dynamic；
Step 3, it rinses, ceramic annulus is placed on deionized water at normal temperature undershoot and is washed till 0.5 minute less；
Step 4, it is dehydrated, ceramic annulus is dehydrated 1 ~ 3 time in dehydrated alcohol:
Step 5, it dries up, the clean compressed air of ceramic annulus is dried up；
Step 6, ceramic annulus is carried out thickness measuring by thickness measuring on calibrator, and nickel layer thickness is controlled in 2mm~10mm range,
Detect the part of unqualified thickness lattice；
Step 7, it post-processes, the ceramic annulus of thickness qualification is put and carries out vacuum heat treatment in a vacuum furnace, at Vacuum Heat
The process conditions of reason: heating rate≤20 DEG C/min, holding temperature are 750 DEG C ~ 850 DEG C, vacuum degree≤10-4Pa, heat preservation terminate
Cool down afterwards with furnace；
Step 8, ceramic annulus is carried out nickel processing, the process conditions of nickelization processing: heating speed by nickel in hydrogen furnace
Rate≤20 DEG C/min, nickel temperature are 900 DEG C ± 10 DEG C, and 5 min -10min of nickel time cools down with furnace after heat preservation, obtains
To the ceramic annulus of the uniform nickel plating in surface, the blistering rate of nickel coating is 0.9%.
Embodiment 2
The present embodiment and the embodiment of embodiment 1 are essentially identical, and the main distinction is, nickel plating part is by 20mm's
The potsherd of the attached molybdenum in surface, the mass percent for plating nickel electrolyte is water 53.5%, nickel sulfate 27.5%, sodium sulphate 9%, magnesium sulfate
5.5%, sodium chloride 0.8% and boric acid 3.7%, the blistering rate of potsherd nickel coating are 1.2%.
Embodiment 3
The present embodiment and the embodiment of embodiment 1 are essentially identical, and the main distinction is, nickel plating part is by 50mm's
The ceramic cylinder of the attached molybdenum in surface, the mass percent for plating nickel electrolyte is water 49.1%, nickel sulfate 30%, sodium sulphate 10%, magnesium sulfate
6%, sodium chloride 0.9% and boric acid 4%, the blistering rate of ceramic cylinder nickel coating are 2.2%.
The present invention is not limited to above-mentioned specific embodiment, person of ordinary skill in the field from the above idea,
Without creative labor, made various transformation are within the scope of the present invention.
Claims (5)
1. a kind of method for reducing ceramic electroless nickel layer blistering, which is characterized in that method includes the following steps:
A. it is surface-treated
Surface of ceramic parts oxidation and pollution condition are estimated, the pickling in acid solution by ceramic part obtains ceramic part I；
B. it is electroplated
Ceramic part I is immersed into nickel plating in nickel bath, obtains ceramic part II；
C. it rinses
Ceramic part II is rinsed with deionized water at normal temperature, obtains ceramic part III；
D. it is dehydrated
Ceramic part III is dehydrated in dehydrated alcohol, obtains ceramic part IV；
E. it dries up
Ceramic part IV is dried up with compressed air, obtains ceramic part V；
F. thickness measuring
Using the nickel layer thickness of calibrator measurement ceramic part V, as nickel layer thickness h < 2mm, step b ~ f is repeated；Work as nickel layer
When thickness 2mm≤h≤10mm, ceramic part VI is obtained, continues subsequent step；As nickel layer thickness h > 10mm, stop working；
G. it post-processes
Ceramic part VI is subjected to vacuum heat treatment in a vacuum furnace, obtains ceramic part VII；The technique of step g vacuum heat treatment
Condition: heating rate≤20 DEG C/min, holding temperature are 750 DEG C ~ 850 DEG C, vacuum degree≤10-4Pa drops after heat preservation with furnace
Temperature；
H. nickel
Ceramic part VII is subjected to nickel processing in hydrogen furnace, obtains required product after nickel.
2. the method according to claim 1 for reducing ceramic electroless nickel layer blistering, it is characterised in that: the step a's
Acid solution is the hydrochloric acid that percent by volume is 30% ~ 50%.
3. the method according to claim 1 for reducing ceramic electroless nickel layer blistering, it is characterised in that: the step b's
The mass percent for plating nickel electrolyte is water 57.8%, nickel sulfate 25%, sodium sulphate 8%, magnesium sulfate 5%, sodium chloride 0.7% and boric acid
3.5%；Or the mass percent of plating nickel electrolyte is water 53.5%, nickel sulfate 27.5%, sodium sulphate 9%, magnesium sulfate 5.5%, chlorination
Sodium 0.8% and boric acid 3.7%；Or the mass percent of plating nickel electrolyte is water 49.1%, nickel sulfate 30%, sodium sulphate 10%, sulfuric acid
Magnesium 6%, sodium chloride 0.9% and boric acid 4%.
4. the method according to claim 1 for reducing ceramic electroless nickel layer blistering, it is characterised in that: the step b plating
The process conditions of nickel: the temperature for plating nickel electrolyte is 35 DEG C ~ 40 DEG C, and the pH value for plating nickel electrolyte is 4.0 ~ 4.5, and current density is
0.8 A/dm2~1.0A/dm2, plating solution keeps flowing during nickel plating.
5. the method according to claim 1 for reducing ceramic electroless nickel layer blistering, it is characterised in that: the step h nickel
Change the process conditions of processing: heating rate≤20 DEG C/min, nickel temperature is 900 DEG C ± 10 DEG C, 5 min of nickel time-
10min cools down after heat preservation with furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610924611.4A CN106435679B (en) | 2016-10-24 | 2016-10-24 | A method of reducing ceramic electroless nickel layer blistering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610924611.4A CN106435679B (en) | 2016-10-24 | 2016-10-24 | A method of reducing ceramic electroless nickel layer blistering |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106435679A CN106435679A (en) | 2017-02-22 |
| CN106435679B true CN106435679B (en) | 2018-12-11 |
Family
ID=58175917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610924611.4A Expired - Fee Related CN106435679B (en) | 2016-10-24 | 2016-10-24 | A method of reducing ceramic electroless nickel layer blistering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106435679B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106534B (en) * | 2019-05-15 | 2021-03-26 | 南京理工大学 | Method for preparing super-hydrophobic nickel surface with wood mirror structure |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392279B (en) * | 2011-10-31 | 2013-10-23 | 成都旭光电子股份有限公司 | Nickel electroplating method of ceramic metalized layer |
| CN105887149B (en) * | 2016-05-27 | 2018-09-25 | 中国电子科技集团公司第五十五研究所 | A kind of metallized ceramic electro-plating method |
-
2016
- 2016-10-24 CN CN201610924611.4A patent/CN106435679B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN106435679A (en) | 2017-02-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI673392B (en) | Anodization architecture for electro-plate adhesion | |
| JP6014807B2 (en) | FUEL CELL SEPARATOR OR FUEL CELL COLLECTING MEMBER AND METHOD FOR PRODUCING THE SAME | |
| CN108570703A (en) | Preparation method of tungsten/copper laminated composite material based on tungsten sheet surface nanocrystallization | |
| CN103382564B (en) | Metal surface superhydrophobic cobalt coating and preparation method thereof | |
| CN108193250A (en) | A kind of sulfuric acid+nitration mixture mixing anode oxidation process | |
| CN107604342B (en) | Metal member, method for manufacturing the same, and processing chamber having the same | |
| CN106637341A (en) | Preparation method for black micro arc oxidation film layers of surfaces of pure aluminum and aluminum alloys | |
| CN102808209B (en) | Method for oxidizing and coloring surfaces of niobium and niobium alloy | |
| CN106011971A (en) | Method for preparing ceramic film/glaze film composite coating on titanium alloy surface | |
| CN106435679B (en) | A method of reducing ceramic electroless nickel layer blistering | |
| CN104532320A (en) | Preparation method of aluminium and titanium alloy micro arc ceramic membrane | |
| CN105316741B (en) | A kind of method for carrying out surface by micro-arc oxidation processing to aluminium alloy using grading current | |
| CN103046073A (en) | Novel composite electrode material of iron base, copper transitional layer and surface nitride coating and preparation method thereof | |
| KR20150014344A (en) | Aluminum alloy member and method of foaming protective film on aluminum alloy | |
| CN103628060B (en) | New electrode materials of molybdenum+depositing titanium nitride and preparation method thereof is oozed on a kind of surface | |
| CN101498024A (en) | Method for preparing ceramic film on titanium alloy surface | |
| CN103820817A (en) | Inner-cooling inert anode for electrolytic aluminum | |
| CN109423675B (en) | Electrolyte for pure aluminum part surface anodic oxidation and pure aluminum part surface anodic oxidation method | |
| CN103540977A (en) | Method for preparing high-gas tightness nickel-copper alloy for travelling wave tube | |
| CN114351203A (en) | Preparation method of ceramic coating on surface of aluminum scroll plate for compressor and scroll plate | |
| CN105200471B (en) | A kind of method of pulse reverse electrodeposition thick tungsten coating | |
| CN201352545Y (en) | Novel tungsten electrode | |
| JP6229771B2 (en) | Fuel cell separator or fuel cell current collector | |
| CN204732430U (en) | A kind of cavity body structure of reaction chamber of solar cell dry method process for etching | |
| CN109440164A (en) | A kind of black ceramic membrane by magnesium alloy differential arc oxidation and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181211 Termination date: 20211024 |