CN104651887A - Process method for plating copper with hydroxyethylidene-1,1-diphosphonic acid (HEDP) - Google Patents
Process method for plating copper with hydroxyethylidene-1,1-diphosphonic acid (HEDP) Download PDFInfo
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- CN104651887A CN104651887A CN201310603283.4A CN201310603283A CN104651887A CN 104651887 A CN104651887 A CN 104651887A CN 201310603283 A CN201310603283 A CN 201310603283A CN 104651887 A CN104651887 A CN 104651887A
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- copper
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- washing
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- 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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a process method for plating copper with hydroxyethylidene-1,1-diphosphonic acid (HEDP). The process method comprises the following steps: polishing and removing oil: polishing a basal body surface and removing oil; performing water-washing: performing water-washing on the oil-removed basal body until the surface is clean and free of impurities; chemically activating and performing water-washing: activating the basal body surface with a chemical activator and performing water-washing until the surface is clean; plating copper: directly placing copper with the hydroxyethylidene-1,1-diphosphonic acid; performing water-washing and acidy copper plating: controlling the concentration of the HEDP to be 160g/L, the concentration of Na2CO3 to be 46.09g/L, the pH value to be 9.0, the Cu<2+> concentration to be 10g/L, the temperature to be 50 DEG C and current density to be 1.5-2A/dm<2>, and performing air stirring; and measuring bonding strength. The process method is simple, and the bonding strength between a copper plating layer and the basal body is measured to be 6418.25N/cm<2>.
Description
(i)
technical fieldthe present invention relates to a kind of process method of plating copper, specifically a kind of hydroxy ethylene diphosphonic acid
(HEDP) process method of plating copper.
(ii)
background technologyhydroxy ethylene diphosphonic acid, be called for short HEDP, sterling is white crystalline powder, molecular weight 206; Soluble in water, be dissolved in methyl alcohol and ethanol.More than 250 DEG C are decomposed.Industrial goods are generally the aqueous solution that content is greater than 50%.It is colourless or pale yellow transparent thick liquid.Relative density (20 DEG C) 1.3 ~ 1.5, pH value (1% aqueous solution) 2.0, phosphorous acid content (in PO3)≤5.0%, ortho-phosphoric acid content (in PO4)≤1.0%, muriate (in Cl)≤1.5%; There is chemical stability, acid-and base-resisting and oxide compound.In water, there is larger dissociation constant, stable complex compound can be formed with iron, copper, aluminium, zinc many kinds of metal ions.The applied research of hydroxy ethylene diphosphonic acid (HEDP) copper-plating technique method is one and has very important scientific meaning and the problem of practical value, it is a kind of efficient complexing agent, it can be formed composite with other complexing agents, make the complex ability of itself and cupric ion close to prussiate, the cathodic polarization of copper electrodeposition is increased, not only inhibits the generation of displacement copper but also fine and close coating can also be obtained.This is not only conducive to cleaner production and the environment protection of electroplating industry, is also conducive to eliminating public safety hidden danger.
(iii) summary of the inventionthe object of the present invention is to provide a kind of hydroxy ethylene diphosphonic acid (HEDP) process method of plating copper.
Hydroxy ethylene diphosphonic acid of the present invention (HEDP) process method of plating copper comprises the steps:
1. polishing oil removing: matrix surface is polished, and oil removing;
2. wash: by the matrix after oil removing with till being washed to clean surface no-sundries;
3. chemical activation, washing: with chemical activating agent matrix surface activated and be washed to clean surface;
4. copper facing: with hydroxy ethylene diphosphonic acid direct copper plating; Control HEDP concentration is 160g/L, Na2CO3 concentration is 46.09g/L, and pH value is 9.0, Cu2+ concentration is 10g/L, and temperature is 50 DEG C, pneumatic blending, and current density is 1.5 ~ 2A/dm2;
5. mensuration copper plate and substrate combinating strength are 6418.25N/cm
2.
The present invention has inquired into best plating solution composition and the processing condition of environment-friendly type HEDP solution system copper facing novel process, and the application of HEDP copper-plating technique on iron-based body.Test that to be have studied by hull trough test with HEDP be the technological process of the alkali plating solution system electro-coppering that the complexing agent of cupric ion and Na2CO3 are conducting salt.By Cu2+ concentration, HEDP/Cu2+, Na2CO3 concentration and pH value four factor in orthogonal experiment discussion plating solution on the impact of plating piece, determine optimum process condition: HEDP concentration is 160g/L, Na2CO3 concentration is 46.09g/L, pH value is 9.0, Cu2+ concentration is 10g/L, temperature is 50 DEG C, pneumatic blending, and current density is 1.5 ~ 2A/dm2.
Embodiment
Hydroxy ethylene diphosphonic acid of the present invention (HEDP) process method of plating copper comprises the steps:
1. polishing oil removing: is polished in copper material surface to be plated, and oil removing;
2. wash: by the copper material after oil removing with till being washed to clean surface no-sundries;
3. chemical activation, washing: with chemical activating agent copper material surface activated and be washed to clean surface;
4. copper facing: with hydroxy ethylene diphosphonic acid direct copper plating; Control HEDP concentration is 160g/L, Na2CO3 concentration is 46.09g/L, and pH value is 9.0, Cu2+ concentration is 10g/L, and temperature is 50 DEG C, pneumatic blending, and current density is 1.5 ~ 2A/dm2;
5. mensuration copper plate and substrate combinating strength are 6418.25N/cm
2.
Claims (1)
1. hydroxy ethylene diphosphonic acid process method of plating copper, is characterized in that comprising the steps:
1. to polish oil removing: matrix surface is polished, and oil removing;
2. wash: by the matrix after oil removing with till being washed to clean surface no-sundries;
3. chemical activation, washing: with chemical activating agent matrix surface activated and be washed to clean surface;
4. copper facing: with hydroxy ethylene diphosphonic acid direct copper plating; Washing, acid copper-plating; Control HEDP concentration is 160g/L, Na2CO3 concentration is 46.09g/L, and pH value is 9.0, Cu2+ concentration is 10g/L, and temperature is 50 DEG C, pneumatic blending, and current density is 1.5 ~ 2A/dm2;
5. mensuration copper plate and substrate combinating strength are 6418.25N/cm
2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310603283.4A CN104651887A (en) | 2013-11-26 | 2013-11-26 | Process method for plating copper with hydroxyethylidene-1,1-diphosphonic acid (HEDP) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310603283.4A CN104651887A (en) | 2013-11-26 | 2013-11-26 | Process method for plating copper with hydroxyethylidene-1,1-diphosphonic acid (HEDP) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104651887A true CN104651887A (en) | 2015-05-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310603283.4A Pending CN104651887A (en) | 2013-11-26 | 2013-11-26 | Process method for plating copper with hydroxyethylidene-1,1-diphosphonic acid (HEDP) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2652328C1 (en) * | 2017-07-06 | 2018-04-25 | Общество с ограниченной ответственностью Производственная компания "НПП СЭМ.М" | Electrolyte for electrolytic deposition of copper |
-
2013
- 2013-11-26 CN CN201310603283.4A patent/CN104651887A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2652328C1 (en) * | 2017-07-06 | 2018-04-25 | Общество с ограниченной ответственностью Производственная компания "НПП СЭМ.М" | Electrolyte for electrolytic deposition of copper |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150527 |