CN113930822A - Electroplating substrate, preparation method thereof and electroplating method - Google Patents
Electroplating substrate, preparation method thereof and electroplating method Download PDFInfo
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- 238000009713 electroplating Methods 0.000 title claims abstract description 158
- 239000000758 substrate Substances 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000007747 plating Methods 0.000 claims abstract description 101
- 230000001681 protective effect Effects 0.000 claims abstract description 72
- 239000003446 ligand Substances 0.000 claims abstract description 56
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000011159 matrix material Substances 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 30
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 26
- 125000004429 atom Chemical group 0.000 claims abstract description 20
- 238000010668 complexation reaction Methods 0.000 claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 62
- 229910052802 copper Inorganic materials 0.000 claims description 55
- 239000010949 copper Substances 0.000 claims description 55
- 238000004528 spin coating Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- -1 imidazole ring compound Chemical class 0.000 claims description 9
- 125000003342 alkenyl group Chemical group 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 10
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 81
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 26
- 229910052710 silicon Inorganic materials 0.000 description 26
- 239000010703 silicon Substances 0.000 description 26
- 235000012431 wafers Nutrition 0.000 description 20
- 230000004888 barrier function Effects 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 230000007547 defect Effects 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 8
- 125000001424 substituent group Chemical group 0.000 description 8
- 238000009736 wetting Methods 0.000 description 7
- 238000011049 filling Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 230000000536 complexating effect Effects 0.000 description 4
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- 125000005017 substituted alkenyl group Chemical group 0.000 description 4
- 125000000547 substituted alkyl group Chemical group 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000004210 cathodic protection Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000752 ionisation method Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 2
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/10—Agitating of electrolytes; Moving of racks
-
- 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
-
- 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
-
- 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
-
- 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
- C25D5/18—Electroplating using modulated, pulsed or reversing current
Landscapes
- 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)
- Electrodes Of Semiconductors (AREA)
Abstract
The application discloses a substrate for electroplating, a preparation method thereof and an electroplating method, belonging to the field of semiconductor processes. The plating base includes: a substrate to be plated and an organic protective film; the surface of the substrate to be plated is provided with a seed layer; the organic protective film is positioned on the surface of the seed layer; the organic protective film includes: and a nitrogen-containing ligand, wherein N atoms in the nitrogen-containing ligand are complexed with metal atoms in the seed layer, and the complexation can be relieved by ionization. The complexation between the organic protective film and the seed layer is combined by virtue of coordination bonds, so that stable binding force is obtained. When the plating base is immersed in the plating solution in an inclined manner, the organic protective film is not damaged by the plating solution due to the bonding force, and the seed layer is effectively protected. Since the complexation can be released by ionization, the organic protective film can be peeled off from the seed layer by applying current to the electroplating matrix for ionization, and the seed layer is exposed, so that the electroplating matrix can carry out normal electroplating operation.
Description
Technical Field
The disclosure relates to the field of semiconductor technology, in particular to a substrate for electroplating, a preparation method thereof and an electroplating method.
Background
Electrochemical copper plating is a common method for obtaining copper interconnection lines in the manufacturing process of integrated circuits at present, and before copper electroplating, a barrier layer needs to be deposited on the surface of a patterned matrix body, such as a silicon wafer, so as to prevent copper from diffusing into a matrix to be plated, and a seed layer of copper is deposited on the surface of the barrier layer for conducting electricity, so as to form the matrix to be plated for electroplating. When copper electroplating is carried out, a substrate to be plated, which is used as a cathode, is inclined at a certain angle into a plating solution, and under the condition that no current is applied, a seed layer on a part of the substrate to be plated, which is in contact with the plating solution first, is dissolved in the plating solution, so that the part cannot be plated with copper normally.
In the related technology, a certain current is applied when a matrix to be plated enters the electroplating solution so as to play a role in cathodic protection and effectively prevent the seed layer which is firstly electroplated in the electroplating solution from being dissolved by the electroplating solution.
In implementing the present disclosure, the inventors found that the related art has at least the following problems:
although the seed layer which is first introduced into the plating solution is cathodically protected in the related art, the seed layer which is not introduced into the plating solution is also applied with current, which easily causes the substrate to be plated to be burnt.
BRIEF SUMMARY OF THE PRESENT DISCLOSURE
In view of the above, the present disclosure provides a substrate for electroplating, a method for preparing the substrate, and an electroplating method, which can solve the above technical problems.
Specifically, the method comprises the following technical scheme:
in one aspect, an embodiment of the present disclosure provides a substrate for electroplating, including: a substrate to be plated and an organic protective film;
the surface of the substrate to be plated is provided with a seed layer;
the organic protective film is positioned on the surface of the seed layer;
the organic protective film includes: a nitrogen-containing ligand, wherein the N atom of the nitrogen-containing ligand complexes with the metal atom of the seed layer, and wherein the complexation is releasable by ionization.
In one possible implementation, the nitrogen-containing ligand is an imidazole ring compound.
In one possible implementation, the chemical structure of the nitrogen-containing ligand is as follows:
wherein R is H, a substituted or unsubstituted alkyl group, or a substituted or unsubstituted alkenyl group.
In one possible implementation, the thickness of the organic protective film is 1nm to 10 nm.
In one possible implementation, the seed layer is a copper seed layer, a cobalt seed layer, or a ruthenium seed layer.
In another aspect, embodiments of the present disclosure provide a method for preparing any one of the above electroplating substrates, where the method includes: providing a substrate to be plated of the surface seed layer;
and forming an organic protective film on the surface of the seed layer to obtain the electroplating matrix.
In one possible implementation manner, the forming the organic protective film on the surface of the seed layer to obtain the plating base includes:
and coating the mixed liquid containing the nitrogen-containing ligand and the acid liquid on the surface of the seed layer of the substrate to be plated, and forming the organic protective film on the surface of the seed layer to obtain the substrate for electroplating.
In a possible implementation manner, the mixed solution is coated on the surface of the seed layer of the substrate to be plated by adopting a spin coating manner, and meanwhile, the spin coating speed is controlled to be 2000rpm-2800 rpm.
In another aspect, an embodiment of the present disclosure provides a method for electroplating any one of the electroplating substrates, including:
dipping the substrate for electroplating into an electroplating solution by inclining a set angle until the substrate for electroplating is completely dipped into the electroplating solution and is kept horizontal;
ionizing the electroplating matrix to remove the complexation between N atoms in the nitrogen-containing ligand and metal atoms in the seed layer, and obtaining the matrix to be plated with the organic protective film removed;
and electroplating the matrix to be plated to form an electroplating layer on the seed layer of the matrix to be plated.
In one possible implementation manner, the ionizing the electroplating substrate to release the complexation between the N atoms in the nitrogen-containing ligand and the metal atoms in the seed layer includes:
applying a first current to the plating base under a first operating condition to perform the ionization treatment;
wherein the first operating condition comprises: the rotation speed of the substrate for electroplating is 10-60 r/min, the flow rate of the electroplating solution is 10-30 l/min, and the current density of the first current is 0.2A/dm2-1A/dm2。
In a possible implementation manner, the electroplating process on the substrate to be plated to obtain an electroplated layer on the seed layer includes:
under a second operation condition, applying a second current to the substrate to be plated to carry out the electroplating treatment;
wherein the second operating condition comprises: the rotation speed of the substrate to be plated is 10-60 r/min, the flow rate of the electroplating solution is 5-20 l/min, and the current density of the second current is 5A/dm2-15A/dm2。
In one possible implementation, the time from the formation of the organic protective film is less than or equal to 2 hours when the plating base is immersed in the plating solution.
The technical scheme provided by the embodiment of the disclosure has the beneficial effects that:
according to the substrate for electroplating provided by the embodiment of the disclosure, a layer of organic protective film is formed on the surface of the seed layer, the organic protective film comprises a nitrogen-containing ligand, N atoms in the nitrogen-containing ligand are complexed with metal atoms in the seed layer, and the organic protective film and the seed layer are combined by virtue of a coordination bond, so that a stable bonding force is obtained. Thus, when the electroplating substrate is obliquely immersed in the electroplating solution, the organic protective film can not be damaged by the electroplating solution based on the binding force, and the seed layer is effectively protected, so that the seed layer which is firstly immersed in the electroplating solution is prevented from being dissolved in advance, and the smooth electroplating operation is ensured. Since the complexation between the N atoms in the nitrogen-containing ligand and the metal atoms in the seed layer can be released by ionization, the organic protective film can be peeled off from the seed layer by applying current to the electroplating matrix for ionization, so that the seed layer is exposed, and the electroplating matrix can be used for normal electroplating operation.
Detailed Description
In order to make the technical solution and advantages of the present disclosure more clear, embodiments of the present disclosure will be described in further detail below.
In the integrated circuit manufacturing process, a conductive network is constructed by copper interconnection lines formed by electrochemical copper plating, and before copper electroplating, a barrier layer is required to be deposited on the patterned surface of a matrix body, such as a silicon wafer, so as to prevent copper from diffusing into a matrix to be plated, and a seed layer of copper is deposited on the surface of the barrier layer for conducting electricity to form the matrix to be plated.
The seed layer on the substrate to be plated is used for forming a conductive surface and promoting the formation and growth of copper crystal nucleus, the thickness of the seed layer is expected to be between 10nm and 40nm and is continuous so as to meet the requirements of a Damascus process, and therefore electroplating can be rapidly carried out on all surfaces of the seed layer to realize super filling from bottom to top. Once the seed layer has defects such as discontinuity or obvious agglomeration, defects such as holes are easily formed in the defect area during electroplating, because the nucleation and growth of copper are stopped at the positions of the holes. Therefore, it is necessary to ensure the continuity of the copper seed layer.
At present, in the copper electroplating, a substrate to be plated as a cathode is immersed in a plating solution in a manner that the substrate is rotated and a seed layer is directed downward, and the substrate to be plated is inclined at a certain angle into the plating solution in order to prevent a large amount of air bubbles from being generated when the substrate to be plated enters the plating solution, which causes the seed layer on a region where the substrate to be plated enters the plating solution to be dissolved in the plating solution (substantially, the copper seed layer is corroded by an acid solution in the plating solution). Until the substrate to be plated is completely immersed in the electroplating solution, the area where the seed layer is dissolved is lack of the seed layer for conducting, so that the electroplating can not be normally carried out, and further, defects such as holes and the like can be generated at the area.
In order to solve the technical problems, in the related art, a certain current is applied while the substrate to be plated enters the electroplating solution to play a role in cathodic protection, so that the seed layer which enters the electroplating solution in advance is effectively prevented from being dissolved by the electroplating solution, but the current is applied to other seed layers which do not enter the electroplating solution at the same time, which is equivalent to being burnt, and the substrate to be plated is easily burnt.
Based on the above technical problem, the embodiments of the present disclosure provide a substrate for electroplating, including: a substrate to be plated and an organic protective film;
the surface of the substrate to be plated is provided with a seed layer;
the organic protective film is positioned on the surface of the seed layer;
the organic protective film includes: and a nitrogen-containing ligand, wherein N atoms in the nitrogen-containing ligand are complexed with metal atoms in the seed layer, and the complexation can be relieved by ionization.
According to the substrate for electroplating provided by the embodiment of the disclosure, a layer of organic protective film is formed on the surface of the seed layer, the organic protective film comprises a nitrogen-containing ligand, N atoms in the nitrogen-containing ligand are complexed with metal atoms in the seed layer, and the organic protective film and the seed layer are combined by virtue of a coordination bond, so that a stable bonding force is obtained. Thus, when the substrate for electroplating is immersed in the electroplating solution in an inclined manner, the organic protective film is not damaged by the electroplating solution based on the bonding force, and the seed layer is effectively protected, so that the seed layer which is firstly immersed in the electroplating solution is prevented from being dissolved (i.e. corroded) in advance, and the smooth electroplating operation is ensured. Since the complexation between the N atoms in the nitrogen-containing ligand and the metal atoms in the seed layer can be released by ionization, the organic protective film can be peeled off from the seed layer by applying current to the electroplating matrix for ionization, so that the seed layer is exposed, and the electroplating matrix can be used for normal electroplating operation.
In addition, as the circuit pattern on the substrate to be plated is finer and finer, the diameter of the through holes to be plated of the circuit pattern is smaller and smaller, for example, the diameter of the through holes to be plated has reached about 2um, air generally exists in the through holes to be plated, and before electroplating, a wetting liquid needs to be sprayed into the through holes to be plated to remove the air existing in the through holes to be plated, so that the electroplating solution can enter the through holes to be plated for electroplating. The process of spraying the wetting liquid into the through hole to be plated is called as a pre-wetting process of the matrix to be plated, and seed layers are arranged on the inner wall of the through hole to be plated and the surface of the matrix to be plated.
At present, the adopted wetting liquid is water, and when the pre-wetting is carried out, one mode is to spray the liquid water, but the mode can cause that the inner part of the through hole to be plated is difficult to be fully wetted, so that the pre-wetting effect is poor. The other method is to spray vapor phase water, however, the vapor phase water is converted into a liquid phase and condensed to the surface of the through hole to be plated by changing parameters such as ambient temperature, air pressure and the like, and the operation is complicated. In addition, the two pre-immersion methods cannot protect the copper seed layer immersed in the plating solution in an uncharged state, and the immersion liquids are easily washed away by the plating solution when entering the plating solution.
According to the embodiment of the disclosure, the organic protective film is arranged on the surface of the seed layer of the to-be-plated substrate, the organic protective film can protect the seed layer, and meanwhile, the organic protective film is positioned on the surface of the whole seed layer, so that the pre-wetting of the to-be-plated through hole in the to-be-plated substrate can be realized, and the electroplating solution can enter the to-be-plated through hole for electroplating. When the seed layer enters the electroplating solution, the organic protective film and the seed layer have complexation and cannot be washed away by the electroplating solution.
In one possible implementation, the nitrogen-containing ligand is an imidazole ring class compound, such as benzimidazole, benzotriazole, and the like. The nitrogen-containing ligand can provide N atoms for complexing with metal atoms, and has the advantages of simple structure, low molecular weight and the like, so that the organic protective film is ensured to enter electroplating solution after being stripped from the seed layer through ionization, the subsequent electroplating operation is not influenced, and the metal plating layer is ensured to have good quality.
In combination with the above implementation manner, for example, the nitrogen-containing ligand is an imidazole ring compound, and the chemical structural formula of the nitrogen-containing ligand is as follows:
wherein R is H, substituted alkyl or unsubstituted alkyl, or substituted alkenyl or unsubstituted alkenyl.
For example, reference to "unsubstituted alkyl" as defined above includes but is not limited to: methyl, ethyl, propyl, butyl, pentyl, hexyl, and the like;
the above "substituted alkyl" refers to an alkyl wherein one hydrogen atom is replaced with a substituent, wherein the substituent includes, but is not limited to: hydroxyl, carboxyl, aldehyde, benzene ring, halogen, etc.
The above "unsubstituted alkenyl" includes, but is not limited to: vinyl, propenyl, allyl, butenyl, pentenyl, and the like.
The above-mentioned "substituted alkenyl" means that one hydrogen atom in the alkenyl group is substituted by a substituent, wherein the substituent includes, but is not limited to: hydroxyl, carboxyl, aldehyde, benzene ring, halogen, etc.
For example, when the seed layer is a copper seed layer, the nitrogen atom in the imidazole ring compound can be complexed with the copper atom in the copper seed layer through a coordination bond, and the complexing process can be shown in the following chemical equation:
in the embodiments of the present disclosure, the organic protective film has a thickness of 1nm to 10nm, for example, 1nm, 2nm, 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, 10nm, etc., and the organic protective film having the above thickness not only can ensure effective protection of the seed layer, but also can be easily peeled off entirely by ionization.
In the embodiment of the disclosure, the substrate to be plated comprises: the substrate comprises a substrate body, a barrier layer and a seed layer; the surface of the matrix body is provided with a line pattern, the barrier layer is positioned on the surface of the line pattern, and the seed layer is positioned on the surface of the barrier layer.
The surface of the base body is provided with a circuit pattern, namely, the circuit pattern is etched on the surface of the base body in advance), and then the metal interconnection line is obtained on the circuit pattern through electroplating. Illustratively, the base body includes, but is not limited to: silicon wafers (also called silicon wafers), resin substrates for printed circuit boards, semiconductor ceramic substrates, and the like.
Before electroplating on the circuit pattern, a barrier layer is required to be formed on the surface of the circuit pattern, and the barrier layer is used for preventing the metal to be plated from diffusing into the matrix body. At present, Ta or TaN is generally deposited on the surface of the circuit pattern of the substrate body by adopting a physical vapor deposition mode to form a barrier layer;
and covering the surface of the barrier layer with a seed layer, for example, depositing the seed layer on the surface of the barrier layer by physical vapor deposition. The seed layer is used to form a conductive surface and promote the formation and growth of metal crystal nuclei to be plated. By way of example, seed layers to which embodiments of the present disclosure relate include, but are not limited to: a copper seed layer, a cobalt seed layer, a ruthenium seed layer, and the like.
When electroplating is carried out, metal to be plated, such as a copper block, is used as an anode, a substrate to be plated is used as a cathode, the anode and the cathode are immersed in electroplating solution, a power supply is connected between the anode and the cathode, the metal to be plated on the anode is subjected to electrochemical reaction and converted into metal ions and electrons, the electrons released by the anode are transferred to the cathode through the electroplating solution, and the metal ions on the surface of the seed layer of the cathode are combined with the electrons released by the anode, so that a plating layer is formed on the surface of the seed layer.
In a possible implementation manner, in the electroplating substrate provided in the embodiments of the present disclosure, the substrate body is a silicon wafer, and the seed layer is a copper seed layer, that is, copper is electroplated on the silicon wafer.
On the other hand, the embodiment of the present disclosure further provides a preparation method of any one of the above electroplating substrates, including: providing a substrate to be plated of the surface seed layer; and
and forming an organic protective film on the surface of the seed layer to obtain the electroplating matrix.
Wherein the organic protective film includes: and a nitrogen-containing ligand, wherein N atoms in the nitrogen-containing ligand are complexed with metal atoms in the seed layer, and the complexation can be relieved by ionization.
In one possible implementation manner, the forming of the organic protective film on the surface of the seed layer to obtain the plating base includes:
and coating the mixed solution containing the nitrogen-containing ligand and the acid solution on the surface of the seed layer of the substrate to be plated, and forming an organic protective film on the surface of the seed layer to obtain the substrate for electroplating.
The coating process is performed at normal temperature, for example, at 20 ℃ to 26 ℃, in the embodiment of the disclosure, the mixed liquid including the nitrogen-containing ligand and the acid liquid is coated on the surface of the seed layer of the substrate to be plated, so that the metal atoms on the seed layer and the nitrogen atoms in the nitrogen-containing ligand form coordinate bonds, the metal atoms and the nitrogen atoms form stable complexes in a matching manner, and the stable complexes continuously extend by taking the coordinate bonds as a unit, so that all the metal atoms on the seed layer are complexed with the nitrogen atoms in the nitrogen-containing ligand, and an organic protective film is formed on the surface of the seed layer to protect the seed layer.
In order to facilitate the above complexation, the nitrogen-containing ligand and the acid solution are mixed to form a mixed solution for coating, and the acid solution is used to provide a reaction solvent for the complexation so that the nitrogen-containing ligand is uniformly dissolved therein, and after the organic protective film is formed, the acid solution can enter the electroplating solution to serve as a base solution of the electroplating solution, thereby avoiding introducing other unnecessary impurities into the electroplating solution.
In addition, based on the above, when the nitrogen-containing ligand and the acid solution are mixed to be used as the mixed solution for coating, the method is very beneficial to the pre-soaking process of the substrate to be plated, and is beneficial to obtaining excellent pre-soaking effect.
The acid is a weak acid such as acetic acid, carbonic acid, etc. to avoid corrosion of the seed layer. The dosage of the acid liquor is controlled to be that the nitrogenous ligand is completely dissolved.
In one possible implementation, the nitrogen-containing ligand is an imidazole-based compound. The above nitrogen-containing ligand not only can provide N atoms for complexing with metal atoms, but also has the advantages of simple structure, low molecular weight, and the like, so that the organic protective film enters the electroplating solution after being stripped from the seed layer by ionization, thereby avoiding introducing undesirable impurities into the electroplating solution and ensuring the platability of the electroplating solution.
In combination with the above implementation manner, for example, the nitrogen-containing ligand is an imidazole ring compound, and the chemical structural formula of the compound is as follows:
wherein R is H, substituted alkyl or unsubstituted alkyl, or substituted alkenyl or unsubstituted alkenyl.
For example, reference to "unsubstituted alkyl" as defined above includes but is not limited to: methyl, ethyl, propyl, butyl, pentyl, hexyl, and the like;
the above "substituted alkyl" refers to an alkyl wherein one hydrogen atom is replaced with a substituent, wherein the substituent includes, but is not limited to: hydroxyl, carboxyl, aldehyde, benzene ring, halogen, etc.
The above "unsubstituted alkenyl" includes, but is not limited to: vinyl, propenyl, allyl, butenyl, pentenyl, and the like.
The above-mentioned "substituted alkenyl" means that one hydrogen atom in the alkenyl group is substituted by a substituent, wherein the substituent includes, but is not limited to: hydroxyl, carboxyl, aldehyde, benzene ring, halogen, etc.
For example, when the seed layer is a copper seed layer, the nitrogen atom in the imidazole ring compound can be complexed with the copper atom in the copper seed layer through a coordination bond, and the complexing process can be shown in the following chemical equation:
in order to make the coating process of the mixture solution more uniform, the embodiment of the disclosure applies the mixture solution to the surface of the seed layer of the substrate to be plated by a spin coating method, and simultaneously, the spin coating speed is controlled to be 2000rpm to 2800rpm, for example, 2050rpm, 2100rpm, 2200rpm, 2300rpm, 2400rpm, 2500rpm, 2600rpm, 2700rpm, 2800rpm, and the like.
In another aspect, embodiments of the present disclosure further provide a method for electroplating a substrate for electroplating, where the method includes:
step 1, dipping the substrate for electroplating into the electroplating solution in an inclined set angle until the substrate for electroplating is totally dipped into the electroplating solution and kept horizontal.
And 2, ionizing the electroplating matrix to remove the complexation between the N atoms in the nitrogen-containing ligand and the metal atoms in the seed layer, thereby obtaining the to-be-plated matrix without the organic protective film.
And 3, electroplating the substrate to be plated to form an electroplated layer on the seed layer of the substrate to be plated.
When the electroplating substrate prepared by the embodiment of the disclosure is subjected to electroplating operation, in the electroplating solution, the organic protective film is firstly stripped from the seed layer by ionization, and the substrate to be plated with the exposed seed layer is obtained. Then, electroplating the substrate to be plated.
When the substrate for electroplating is immersed in the electroplating solution, namely, when the step 1 is carried out, the time for carrying out the step 1 is less than or equal to 2 hours away from the formation time of the organic protective film, so that the continuity and the integrity of the organic protective film can be ensured, and the protective effect on the seed layer is improved.
The above steps are described as follows:
in step 1, the plating substrate is immersed in the plating solution while rotating with the seed layer facing downward, and the plating substrate is tilted at a predetermined angle while being immersed in the plating solution, so as to prevent the plating substrate from generating a large amount of bubbles when entering the plating solution. Wherein the inclination angle is less than or equal to 7 DEG, for example, 4 DEG, 5 DEG, 6 DEG or the like, as measured from the angle between the plating base and the horizontal plane. After the entire substrate for plating is immersed in the plating solution and kept horizontal, step 2 is performed.
And 2, ionizing the electroplating matrix to remove the complexation between the N atoms in the nitrogen-containing ligand and the metal atoms in the seed layer, thereby obtaining the to-be-plated matrix from which the organic protective film is removed.
The seed layer is used as a copper seed layer, the nitrogen-containing ligand is an imidazole ring compound, for example, ionization between nitrogen atoms in the imidazole ring compound and copper atoms in the copper seed layer is relieved through ionization, and the ionization process can be seen in the following chemical equation:
it can be seen that after ionization, the organic protective film is peeled off from the copper seed layer, the copper seed layer is exposed, and copper atoms on the copper seed layer serve as a seed to facilitate the growth of a copper plating layer thereon.
In order to make the above ionization smoothly proceed, that is, only the organic protective film can be peeled off without plating occurring, the embodiment of the present disclosure exemplifies that the ionization treatment is performed by applying the first current to the substrate for plating under the first operation condition.
Wherein the first operating condition comprises: the rotation speed of the substrate for electroplating is 10-60 r/min, the flow rate of the electroplating solution is 10-30L/min, and the current density of the first current is 0.2A/dm2-1A/dm2。
For example, the rotation speed of the plating base includes, but is not limited to: 10 rpm, 20 rpm, 30 rpm, 40 rpm, 50rpm, 60 rpm, etc.;
the flow rates of the plating solution during the ionization process include, but are not limited to: 10, 15, 20, 25, 30, etc.;
the density of the first current applied to the plating base includes, but is not limited to: 0.2A/dm2、0.3A/dm2、0.4A/dm2、0.5A/dm2、0.6A/dm2、0.7A/dm2、0.8A/dm2、0.9A/dm2Etc.;
the time for the ionization treatment is 3 seconds to 30 seconds, including, but not limited to: 5 seconds, 10 seconds, 15 seconds, 20 seconds, 25 seconds, 30 seconds, etc. The ionization time is determined by the thickness of the organic protective film, and the thicker the organic protective film, the longer the ionization time, and the ionization time is controlled to be 3 seconds to 30 seconds based on the thickness of the organic protective film being 1nm to 10nm in the disclosed embodiment.
Under the first operating condition, the ionization can be smoothly and sufficiently performed, the organic protective film is sufficiently peeled off, the entire seed layer is exposed, and the plating does not occur after the seed layer is exposed under the first current having the current density. The substrate to be plated is electroplated by continuing to increase the current density and changing other operating conditions, see step 3.
And 3, performing electroplating treatment on the substrate to be plated to form an electroplating layer on the seed layer of the substrate to be plated.
In order to make the electroplating process smoothly proceed, the embodiment of the disclosure exemplifies that the electroplating treatment is performed by applying a second current to the substrate to be plated on which the seed layer is exposed under the second operation condition.
Wherein the second operating condition comprises: the rotation speed of the substrate to be plated is 10-60 rpm, the flow rate of the plating solution is 5-20L/min, and the current density of the second current is 5A/dm2-15A/dm2。
For example, the rotation speed of the substrate to be plated includes, but is not limited to: 10 rpm, 20 rpm, 30 rpm, 40 rpm, 50rpm, 60 rpm, etc.;
the flow rates of the plating solution during the plating process include, but are not limited to: 5 liters/minute, 10 liters/minute, 15 liters/minute, 20 liters/minute, and the like;
the density of the second current applied to the substrate to be plated includes, but is not limited to: 5A/dm2、8A/dm2、10A/dm2、12A/dm2、13A/dm2、14A/dm2、15A/dm2Etc.;
the time of the plating treatment is 10 seconds to 500 seconds, including but not limited to: 10 seconds, 50 seconds, 100 seconds, 200 seconds, 250 seconds/300 seconds, 350 seconds, 400 seconds, 450 seconds, etc. The time of the electroplating treatment is determined by the thickness of the metal coating, the thicker the metal coating is, the longer the electroplating treatment is, and the time of the electroplating treatment is controlled to be 10-500 seconds according to the current requirement on the thickness of the metal coating. For example, if a copper plating layer with a thickness of 1 μm is to be plated, the plating time is about 120 seconds.
Under the second operation condition, electroplating can be rapidly and sufficiently carried out on all the surfaces of the seed layer, super filling from bottom to top is realized, and the defects of discontinuity and the like of the seed layer are avoided. The current density used in the plating operation is significantly increased compared to the current density used in the ionization operation. Therefore, when the electroplating substrate is electroplated, the small current is firstly conducted for ionization, and then the large current is conducted for electroplating, each operation process is independently conducted, smoothness and continuity are achieved (namely, the ionization operation and the electroplating operation are compatible), the operation is simple, and the preparation cost is low.
In a possible implementation manner, in the electroplating substrate provided by the embodiment of the disclosure, the substrate body used is a silicon wafer, and the metal to be plated is copper, that is, a method for electroplating copper on the silicon wafer is provided.
The electroplating method according to the embodiment of the present disclosure can be applied to the following scenarios, but not limited to: electroplating in the chip field, electroplating in the package field, electroplating in the printed circuit board field, and the like.
The present disclosure will be further described below by specific examples.
Example 1
The present embodiment provides a base for plating, comprising: the silicon chip comprises a substrate to be plated and an organic protective film, wherein the substrate to be plated is a silicon chip with a copper seed layer on the surface, the organic protective film comprises a nitrogen-containing ligand, and N atoms in the nitrogen-containing ligand are complexed with copper atoms in the seed layer. The chemical structure of the nitrogen-containing ligand is shown as follows:
the matrix for electroplating is prepared by the following method:
at the temperature of 25 ℃, the nitrogen-containing ligand is fully dissolved in acetic acid, and the mixture is stirred and mixed into uniform mixed liquid. The mixture was applied to a copper seed layer of a silicon wafer by spin coating, the flow rate of the mixture during spin coating was controlled to 1.8sccm (i.e., 1.8 ml/min), the spin coating rotation speed was controlled to 2500rpm, and a 2nm thick organic protective film was formed on the copper seed layer, thereby obtaining a substrate for plating as desired in the present example.
The electroplating matrix is electroplated by adopting the following method:
and obliquely immersing the electroplating substrate into the electroplating solution at an included angle of 5 degrees with the horizontal direction until the electroplating substrate is completely immersed into the electroplating solution and is kept horizontal.
Under a first operation condition, a first current is applied to the matrix for electroplating to carry out ionization treatment, and a matrix to be plated, namely a silicon wafer with a copper seed layer on the surface is obtained. Wherein the first operating condition comprises: the rotation speed of the plating base was 30 rpm, the flow rate of the plating solution was 15 liters/min, and the current density of the first current was 0.5A/dm2The time for the ionization treatment was 10 seconds.
And under a second operation condition, applying a second current to the silicon wafer with the copper seed layer on the surface to carry out electroplating treatment, so as to obtain a copper plating layer on the silicon wafer. Wherein the second operating condition comprises: the rotation speed of the substrate to be plated is 25 rpm, the flow rate of the plating solution is 10 liters/min, and the current density of the second current is 10A/dm2The time for the plating treatment was 150 seconds.
The test result shows that the electroplating can be rapidly and fully carried out on all the surfaces of the seed layer, the super filling from bottom to top is realized, and the obtained plating layer has uniform texture and does not have defects such as holes, cracks and the like.
Example 2
The present embodiment provides a base for plating, comprising: the silicon chip comprises a substrate to be plated and an organic protective film, wherein the substrate to be plated is a silicon chip with a copper seed layer on the surface, the organic protective film comprises a nitrogen-containing ligand, and N atoms in the nitrogen-containing ligand are complexed with copper atoms in the seed layer. The chemical structure of the nitrogen-containing ligand is shown as follows:
the matrix for electroplating is prepared by the following method:
at the temperature of 25 ℃, the nitrogen-containing ligand is fully dissolved in acetic acid, and the mixture is stirred and mixed into uniform mixed liquid. The mixed solution was applied to a copper seed layer of a silicon wafer by spin coating, the flow rate of the mixed solution during spin coating was controlled to 2sccm, the spin coating rotation speed was controlled to 2000rpm, and a 5nm thick organic protective film was formed on the copper seed layer to obtain a substrate for plating as desired in the present example.
The electroplating matrix is electroplated by adopting the following method:
the substrate for plating was immersed in the plating solution with an inclination of 6 ° from the horizontal until the substrate for plating was completely immersed in the plating solution and kept horizontal.
Under a first operation condition, a first current is applied to the matrix for electroplating to carry out ionization treatment, and a matrix to be plated, namely a silicon wafer with a copper seed layer on the surface is obtained. Wherein the first operating condition comprises: the rotation speed of the plating base was 40 rpm, the flow rate of the plating solution was 20 liters/min, and the current density of the first current was 0.8A/dm2The time for the ionization treatment was 20 seconds.
And under a second operation condition, applying a second current to the silicon wafer with the copper seed layer on the surface to carry out electroplating treatment, so as to obtain a copper plating layer on the silicon wafer. Wherein the second operating condition comprises: the rotation speed of the substrate to be plated was 40 rpm, the flow rate of the plating solution was 5 liters/min, and the current density of the second current was 12A/dm2The time for the plating treatment was 300 seconds.
The test result shows that the electroplating can be rapidly and fully carried out on all the surfaces of the seed layer, the super filling from bottom to top is realized, and the obtained plating layer has uniform texture and does not have defects such as holes, cracks and the like.
Example 3
The present embodiment provides a base for plating, comprising: the silicon chip comprises a substrate to be plated and an organic protective film, wherein the substrate to be plated is a silicon chip with a copper seed layer on the surface, the organic protective film comprises a nitrogen-containing ligand, and N atoms in the nitrogen-containing ligand are complexed with copper atoms in the seed layer. The chemical structure of the nitrogen-containing ligand is shown as follows:
the matrix for electroplating is prepared by the following method:
the nitrogen-containing ligand is fully dissolved in carbonic acid at the temperature of 25 ℃, and the mixture is stirred and mixed into uniform mixed liquid. The mixed solution was applied to a copper seed layer of a silicon wafer by spin coating, the flow rate of the mixed solution during spin coating was controlled to 2sccm, the spin coating rotation speed was controlled to 2800rpm, and a 10nm thick organic protective film was formed on the copper seed layer to obtain a substrate for plating as desired in the present example.
The electroplating matrix is electroplated by adopting the following method:
the substrate for plating is immersed into the plating solution with an angle of 4 DEG with respect to the horizontal direction until the substrate for plating is completely immersed into the plating solution and kept horizontal.
Under a first operation condition, a first current is applied to the matrix for electroplating to carry out ionization treatment, and a matrix to be plated, namely a silicon wafer with a copper seed layer on the surface is obtained. Wherein the first operating condition comprises: the rotation speed of the plating base was 60 rpm, the flow rate of the plating solution was 30 liters/min, and the current density of the first current was 1A/dm2The time for the ionization treatment was 30 seconds.
And under a second operation condition, applying a second current to the silicon wafer with the copper seed layer on the surface to carry out electroplating treatment, so as to obtain a copper plating layer on the silicon wafer. Wherein the second operating condition comprises: to-be-plated baseThe rotating speed of the body was 60 rpm, the flow rate of the plating solution was 20 liters/min, and the current density of the second current was 15A/dm2The time for the plating treatment was 400 seconds.
The test result shows that the electroplating can be rapidly and fully carried out on all the surfaces of the seed layer, the super filling from bottom to top is realized, and the obtained plating layer has uniform texture and does not have defects such as holes, cracks and the like.
The above description is only for facilitating the understanding of the technical solutions of the present disclosure by those skilled in the art, and is not intended to limit the present disclosure. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
Claims (12)
1. A plating base, comprising: a substrate to be plated and an organic protective film;
the surface of the substrate to be plated is provided with a seed layer;
the organic protective film is positioned on the surface of the seed layer;
the organic protective film includes: a nitrogen-containing ligand, wherein the N atom of the nitrogen-containing ligand complexes with the metal atom of the seed layer, and wherein the complexation is releasable by ionization.
2. A plating substrate according to claim 1, wherein the nitrogen-containing ligand is an imidazole ring compound.
3. A plating substrate according to claim 2, wherein the nitrogen-containing ligand has a chemical formula shown below:
wherein R is H, a substituted or unsubstituted alkyl group, or a substituted or unsubstituted alkenyl group.
4. A plating substrate according to claim 1, wherein the organic protective film has a thickness of 1nm to 10 nm.
5. A plating substrate according to claim 1, wherein the seed layer is a copper seed layer, a cobalt seed layer, or a ruthenium seed layer.
6. A method for producing a plating substrate according to any one of claims 1 to 5, characterized by comprising: providing a substrate to be plated of the surface seed layer;
and forming an organic protective film on the surface of the seed layer to obtain the electroplating matrix.
7. The method according to claim 6, wherein the step of forming the organic protective film on the surface of the seed layer to obtain the plating base comprises:
and coating the mixed liquid containing the nitrogen-containing ligand and the acid liquid on the surface of the seed layer of the substrate to be plated, and forming the organic protective film on the surface of the seed layer to obtain the substrate for electroplating.
8. The method according to claim 7, wherein the mixture is applied to the surface of the seed layer of the substrate by spin coating, and the spin coating speed is controlled to be 2000rpm to 2800 rpm.
9. A method of electroplating a substrate according to any of claims 1 to 5, comprising:
dipping the substrate for electroplating into an electroplating solution by inclining a set angle until the substrate for electroplating is completely dipped into the electroplating solution and is kept horizontal;
ionizing the electroplating matrix to remove the complexation between N atoms in the nitrogen-containing ligand and metal atoms in the seed layer, and obtaining the matrix to be plated with the organic protective film removed;
and electroplating the matrix to be plated to form an electroplating layer on the seed layer of the matrix to be plated.
10. A plating method of a plating substrate according to claim 9, wherein said ionizing treatment of the plating substrate to release the complexation between the N atoms in the nitrogen-containing ligand and the metal atoms in the seed layer comprises:
applying a first current to the plating base under a first operating condition to perform the ionization treatment;
wherein the first operating condition comprises: the rotation speed of the substrate for electroplating is 10-60 r/min, the flow rate of the electroplating solution is 10-30 l/min, and the current density of the first current is 0.2A/dm2-1A/dm2。
11. The method of plating a substrate for plating according to claim 9, wherein said subjecting the substrate to be plated to a plating treatment to obtain a plating layer on said seed layer comprises:
under a second operation condition, applying a second current to the substrate to be plated to carry out the electroplating treatment;
wherein the second operating condition comprises: the rotation speed of the substrate to be plated is 10-60 r/min, the flow rate of the electroplating solution is 5-20 l/min, and the current density of the second current is 5A/dm2-15A/dm2。
12. A plating method for a plating base according to claim 9, characterized in that a time to form said organic protective film is 2 hours or less when said plating base is immersed in said plating solution.
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| CN117328113A (en) * | 2023-10-16 | 2024-01-02 | 广东省广新离子束科技有限公司 | Acid copper plating process for metallized film and application |
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