CN111041533B - Electroplating solution for electroplating pure cobalt and application thereof - Google Patents
Electroplating solution for electroplating pure cobalt and application thereof Download PDFInfo
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- CN111041533B CN111041533B CN201911423782.9A CN201911423782A CN111041533B CN 111041533 B CN111041533 B CN 111041533B CN 201911423782 A CN201911423782 A CN 201911423782A CN 111041533 B CN111041533 B CN 111041533B
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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
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/76877—Filling of holes, grooves or trenches, e.g. vias, with conductive material
- H01L21/76879—Filling of holes, grooves or trenches, e.g. vias, with conductive material by selective deposition of conductive material in the vias, e.g. selective C.V.D. on semiconductor material, plating
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76898—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics formed through a semiconductor substrate
Abstract
The invention provides an electroplating solution for electroplating pure cobalt and application thereof, wherein the electroplating solution for electroplating pure cobalt comprises the following components: a base solution, which is an aqueous solution of a soluble cobalt salt; a complexing agent comprising a conjugated oxime group. According to the electroplating solution for electroplating pure cobalt, the complexing agent of the conjugated oxime group is used, so that the strong cathode polarization effect is achieved on the electrochemical deposition of cobalt ions, the deposition rate of cobalt can be controlled, the cobalt can be uniformly nucleated and grown, a high-quality pure cobalt coating is obtained, and the electrical interconnection is achieved.
Description
Technical Field
The invention relates to the technical field of applied electrochemistry, in particular to an electroplating solution for electroplating pure cobalt and application thereof.
Background
The desire for reduced size and improved performance of electronic devices has driven the development of interconnect technology towards smaller interconnect feature sizes, so that more components can be integrated in a more limited electronic area. As feature sizes shrink, more and more problems arise, such as electromigration, interdiffusion, and the like.
Currently, the interconnect is mainly realized by electroplating copper. However, since copper has a non-negligible electromigration and the problem becomes more and more prominent as the size of the interconnect becomes smaller, a material for realizing the interconnect instead of electrolytic copper plating is urgently required to be developed.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a die interconnect material capable of realizing an interconnect size of 7nm or less.
The inventors of the present invention have repeatedly studied and found that if cobalt is used as an interconnect material, the following advantages are present compared to copper:
(1) cobalt is more difficult to diffuse in silicon than copper, thereby reducing electromigration, and cobalt metallization provides a complete gap fill without the need for high resistance thin barrier layers (or barriers, usually tantalum nitride, titanium nitride, etc., for copper, such barriers are needed to reduce copper diffusion into silicon);
(2) cobalt can have lower resistance in chip packages because a high resistance barrier layer is not needed, and as chip package size decreases, the high resistance thin layer contributes more and more to resistance. Overall, therefore, as chip package sizes decrease, cobalt metal can instead achieve lower resistance in the package than copper; (3) the full metal cobalt realizes electroplating filling, and has no gap, no seam and no filler, so that the manufactured chip silicon is in thermal matching with metal or has better thermal conductivity.
Therefore, the cobalt material is used to replace the copper material, and the cobalt material is used as a chip interconnection material, which is a great revolutionary update.
However, the problem of how to control the deposition rate of cobalt is an urgent problem to be solved in electroplating pure cobalt. The inventors repeatedly research and find that the deposition rate of cobalt can be well controlled by adding a proper complexing agent, the packaging of a chip is realized, and the invention is completed on the basis.
The invention provides an electroplating solution for electroplating pure cobalt on one hand.
The invention also provides the application of electroplating for electroplating pure cobalt in the field of chip packaging.
In order to solve the technical problems, the invention adopts the following technical scheme:
according to a first aspect of the present invention, there is provided an electroplating solution for electroplating pure cobalt, comprising:
a base solution, which is an aqueous solution of a soluble cobalt salt;
a complexing agent comprising a conjugated oxime group.
Further, the soluble cobalt salt comprises one or more of hydrated cobalt sulfate, hydrated cobalt chloride and hydrated cobalt nitrate, and the concentration of the soluble cobalt salt in the base solution is 0.02-0.4M.
Further, the electroplating solution for electroplating pure cobalt also contains 0.1-0.6M boric acid, and the pH value of the electroplating solution for electroplating pure cobalt is 3.0-5.0.
Further, the complexing agent is one or more of dimethylglyoxime, 1, 2-cyclohexanedione dioxime and cyclohexanone oxime.
Further, the concentration of the complexing agent is 500-40000 ppm.
Further, the electroplating solution for electroplating pure cobalt also contains additives, wherein the additives comprise one or more of wetting agents, brightening agents and accelerating agents.
Furthermore, the wetting agent is sodium dodecyl sulfate, and the concentration of the wetting agent is 0.08-0.12 g/L.
Further, the brightening agent is saccharin sodium, sodium sulfate or a mixture of saccharin sodium and sodium sulfate, and the concentration of the brightening agent is 0.05-0.2M.
Further, the accelerator is 2-mercaptobenzimidazole-5-sodium sulfonate dihydrate, and the concentration of the accelerator is 0-300 mu mol/L.
According to a second aspect of the invention, the application of the electroplating solution for electroplating pure cobalt in chip packaging is also provided.
The technical scheme of the invention at least has one of the following beneficial effects:
according to the electroplating solution for electroplating pure cobalt, the complexing agent of the conjugated oxime group is used, so that the strong cathode polarization effect is achieved on the electrochemical deposition of cobalt ions, the deposition rate of cobalt can be controlled, the cobalt can uniformly nucleate and grow, a high-quality pure cobalt coating is obtained, and the electrical interconnection is achieved;
by replacing pure copper electroplating with pure cobalt electroplating, the risk of electromigration and interdiffusion can be reduced.
Drawings
FIG. 1 is a schematic view of an electroplating apparatus for electroplating with an electroplating solution for electroplating pure cobalt according to an embodiment of the present invention;
FIG. 2 is a photograph of a cut piece after pure cobalt electroplating using the electroplating solution according to example 1 of the present invention;
FIG. 3 is a photograph of a cut piece after pure cobalt electroplating according to example 2 was performed using the electroplating solution.
Description of reference numerals:
1, a direct current power supply; 2, conducting wires; 3, electroplating bath; 4TSV through silicon via samples (cathodes); 5, nitrogen bubbles; 6 electroplating solution; 7, stirring the flowing direction of the plating solution by nitrogen to show a curve; 8 nitrogen pipeline and nozzle; 9 pure cobalt anode.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few 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 described embodiments of the invention, are within the scope of the invention.
First, an electroplating solution for electroplating pure cobalt according to an embodiment of the present invention will be described in detail.
The electroplating solution for electroplating pure cobalt according to the embodiment of the invention comprises a base solution and a complexing agent.
Wherein the base solution is an aqueous solution of a soluble cobalt salt.
The soluble cobalt salt can be selected from one or more of hydrated cobalt sulfate, hydrated cobalt chloride and hydrated cobalt nitrate, and the concentration of the soluble cobalt salt can be 0.02-0.4M.
Further, considering the presence of a large amount of chlorine gas, it is preferable that hydrated cobalt sulfate, hydrated cobalt nitrate, or a mixture thereof is used, since gas is easily generated during plating to deteriorate the quality of the plating layer.
Wherein the electroplating solution for electroplating pure cobalt can also contain 0.1-0.6M boric acid.
The boric acid not only can play a role in stabilizing the pH value, but also can expand the bright current density range of the cathode, and ensure that the coating is crystallized and fine, improve the ductility of the coating and enhance the binding force between the coating and a substrate.
The pH of the plating solution for plating pure cobalt is preferably 3.0 to 5.0, and may be specifically adjusted using sulfuric acid, nitric acid, sodium hydroxide, potassium hydroxide, or the like.
The complexing agent can effectively adjust the deposition rate of cobalt as long as the complexing agent has conjugated oxime groups, so that a high-quality pure cobalt coating is obtained. Preferably, the complexing agent may be one or more of dimethylglyoxime, 1, 2-cyclohexanedione dioxime and cyclohexanone oxime.
Wherein, the chemical structural formula of the dimethylglyoxin Dimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyldimethyloxime (DMG) is shown as the following formula (1):
when the dimethylglyoxime is used, the concentration range of an electroplating solution for electroplating pure cobalt can be 10000-40000 ppm.
The chemical structural formula of the 1, 2-cyclohexanedione dioxime (CHD cyclohexane dioxime) is shown as the following formula (2):
when the 1, 2-cyclohexanedione dioxime is used, the concentration range of the electroplating solution for electroplating pure cobalt can be 3000-7000 ppm.
The chemical structural formula of the cyclohexanone oxime (CHO cyclohexane oxide) is shown as the following formula (3):
the concentration of the cyclohexanone oxime in an electroplating solution for electroplating pure cobalt can be 500-1000 ppm.
The 3 kinds of complexing agents may be used alone or in combination of two or more. When a plurality of kinds are used in combination, the content of each plating solution for plating pure cobalt can be appropriately adjusted depending on the equivalent concentration of the conjugated oxime group.
The plating solution for pure cobalt plating may contain various additives as needed in addition to the base solution and the complexing agent, and as the additives, for example, one or more of a wetting agent, a brightener, and an accelerator may be cited.
The wetting agent can be sodium dodecyl sulfate, and the concentration of the wetting agent in the electroplating solution for electroplating pure cobalt can be 0.08-0.12 g/L, for example.
The brightener can be saccharin sodium, sodium sulfate or a mixture thereof, and the concentration of the brightener can be 0.05-0.2M.
The accelerator can be 2-mercaptobenzimidazole-5-sodium sulfonate dihydrate, and the concentration of the accelerator can be 0-300 mu mol/L.
Hereinafter, the electroplating solution for electroplating pure cobalt and the application thereof in the field of chip packaging will be described in further detail with reference to specific examples.
Example 1
The electroplating solution for electroplating pure cobalt comprises the following components in percentage by weight and pH value:
base solution: CoSO4.7H2O，80g/L
CoCl2.6H2O，10g/L
Boric acid: h3BO3,20g/L
pH value: pH 4
Wetting agent: sodium Dodecyl Sulfate (SDS), 1.0g/L
Brightening agent: saccharin sodium, 1.0g/L
Accelerator: 2 mercapto benzimidazole-5-sodium sulfonate dihydrate (MBIS), 0.050g/L
Complexing agent: dimethylglyoxime (DMG), 20000 ppm.
Specifically, firstly weighing CoSO4.7H2O、CoCl2.6H2Adding O into water, stirring, and adding boric acid after the O is fully dissolved. Then, the wetting agent, the brightening agent, the accelerator and the complexing agent are gradually added, the mixture is fully stirred, and the pH value is adjusted to 4 through sulfuric acid and sodium hydroxide, so that the electroplating solution for electroplating pure cobalt is obtained.
In order to evaluate the effect of using the plating solution for plating pure cobalt of the present invention, a silicon wafer having through-silicon vias (TSVs) was plated using the same. Specifically, a sample is rinsed and vacuumized, then the sample is arranged in an electroplating bath according to the schematic diagram of the device shown in fig. 1, pure nitrogen is started to stir, the stirring intensity of the nitrogen is 1.0-2.0L/min, and electroplating is carried out, wherein the electroplating conditions are as follows: current density 1ASD, plating time 66 min.
And (3) selecting a sample with a TSV (through silicon via) area from the electroplated sample to prepare a slice, then grinding and polishing, and observing whether the TSV in the section is completely filled with metal or not. The results are shown in FIG. 2 without any significant voids (i.e., voids having a diameter in excess of 1 um).
Example 2
The electroplating solution for electroplating pure cobalt comprises the following components in percentage by weight and pH value:
base solution: CoSO4.7H2O，60g/L
CoCl2.6H2O，10g/L
Boric acid: h3BO3, 30g/L
pH value: pH 5
Wetting agent: SDS, 1.2g/L
Brightening agent: saccharin sodium, 0.8g/L
Accelerator: MBIS, 0.030g/L
Complexing agent: cyclohexanone oxime (CHO), 1000ppm
The specific production method is the same as in example 1, and the description thereof is omitted.
In order to evaluate the effect of using the plating solution for plating pure cobalt of the present invention, a Through Silicon Via (TSV) sample was plated using the same. Specifically, a sample is rinsed and vacuumized, then the sample is arranged in an electroplating bath according to the schematic diagram of the device shown in fig. 1, pure nitrogen is started to stir, the stirring intensity of the nitrogen is 1.0-2.0L/min, and electroplating is carried out, wherein the electroplating conditions are as follows: the current density was 0.8ASD, and the plating time was 83 min.
And (3) selecting a sample with a TSV (through silicon via) area from the electroplated sample to prepare a slice, then grinding and polishing, and observing whether the TSV in the section is completely filled with metal or not. The results are shown in FIG. 3 without any significant voids (i.e., voids having a diameter in excess of 1 um).
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. An electroplating solution for electroplating pure cobalt, comprising:
a base solution, which is an aqueous solution of a soluble cobalt salt;
a complexing agent comprising a conjugated oxime group,
the electroplating solution for electroplating pure cobalt also contains 0.1-0.6M boric acid, the pH value of the electroplating solution for electroplating pure cobalt is 4.0,
the complexing agent is one of dimethylglyoxime, 1, 2-cyclohexanedione dioxime and cyclohexanone oxime,
when the dimethylglyoxime is used, the concentration range of the electroplating solution for electroplating pure cobalt is 10000-40000 ppm,
when the 1, 2-cyclohexanedione dioxime is used, the concentration range of the electroplating solution for electroplating pure cobalt is 3000-7000 ppm,
when the cyclohexanone oxime is used, the concentration range of the electroplating solution for electroplating pure cobalt is 500-1000 ppm.
2. The plating solution for plating pure cobalt according to claim 1, wherein the soluble cobalt salt comprises one or more of cobalt sulfate hydrate, cobalt chloride hydrate, and cobalt nitrate hydrate, and the concentration of the soluble cobalt salt in the base solution is 0.02 to 0.4M.
3. The plating solution for electroplating pure cobalt according to claim 1, further comprising an additive, wherein the additive comprises one or more of a wetting agent, a brightener and an accelerator.
4. The plating solution for plating pure cobalt according to claim 3,
the wetting agent is sodium dodecyl sulfate, and the concentration of the wetting agent is 0.08-0.12 g/L.
5. The plating solution for plating pure cobalt according to claim 3,
the brightener is saccharin sodium, sodium sulfate or a mixture of saccharin sodium and sodium sulfate, and the concentration of the brightener is 0.05-0.2M.
6. The plating solution for plating pure cobalt according to claim 5,
the accelerator is a 2-mercaptobenzimidazole-5-sodium sulfonate dihydrate, and the concentration of the accelerator is 0-300 mu mol/L.
7. Use of the electroplating solution for electroplating pure cobalt according to any one of claims 1 to 6 in chip packaging.
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| CN113106506A (en) * | 2021-04-15 | 2021-07-13 | 电子科技大学 | Plating solution for electroplating cobalt and electroplating method |
| CN114940740B (en) * | 2022-06-29 | 2023-04-21 | 华南理工大学 | High-performance transparent room-temperature self-repairing polyurethane elastomer based on multiple reversible actions and preparation method thereof |
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