CN103700619B - Copper-connection is electroplated fill method - Google Patents
Copper-connection is electroplated fill method Download PDFInfo
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- CN103700619B CN103700619B CN201310697825.9A CN201310697825A CN103700619B CN 103700619 B CN103700619 B CN 103700619B CN 201310697825 A CN201310697825 A CN 201310697825A CN 103700619 B CN103700619 B CN 103700619B
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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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- 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
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/425—Plated through-holes or plated via connections characterised by the sequence of steps for plating the through-holes or via connections in relation to the conductive pattern
- H05K3/426—Plated through-holes or plated via connections characterised by the sequence of steps for plating the through-holes or via connections in relation to the conductive pattern initial plating of through-holes in substrates without metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2221/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof covered by H01L21/00
- H01L2221/10—Applying interconnections to be used for carrying current between separate components within a device
- H01L2221/1068—Formation and after-treatment of conductors
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- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention relates to a kind of copper-connection and electroplate fill method, comprise the following steps: using the copper plating bath of filling for hole as electrolyte, put into three-electrode system, measure its electrochemistry curve; Determine current peak and magnitude of voltage corresponding to electric current paddy difference according to electrochemistry curve; The sample with pore structure is put into three-electrode system as working electrode, make the voltage of hole surface corresponding to voltage corresponding to electric current paddy on electrochemistry curve, after energising, take out; The thickness of copper is filled in measured hole cross section everywhere, and its thickness is corresponding to the position of current peak on electrochemistry curve; Adjust the concentration of copper plating bath, change the position of current peak and electric current paddy on its electrochemistry curve, make the voltage of hole surface in electro-coppering process corresponding to voltage corresponding to electric current paddy on electrochemistry curve, the voltage at the bottom of hole is corresponding to voltage corresponding to current peak on electrochemistry curve. The present invention can realize flawless perfect filling of copper facing, and easy and simple to handle, can be widely used in various high-end electronic manufacturing fields.
Description
Technical field
The present invention relates to a kind of method of electroplating filling, be specifically related to a kind of copper-connection and electroplate the method for filling.
Background technology
In Electronic Encapsulating Technology, the copper facing technology of hole or metallic channel is the focus that researcher pays close attention to always. Itself and common copper facing technology have a great difference, and its difficult point is to ensure copper preferential deposition in hole, complete in a short period of time seamless, fill without hole, reach " bottom-up " (bottom-up) filling effect. So-called " bottom-up " filling is the sedimentation rate that the sedimentation rate at the bottom of finger-hole is greater than aperture, just can form this filling forms and only add multiple additives in electroplate liquid. Electroplate and fill for the copper in hole, researcher has taked kinds of schemes to be optimized, for example, adopt positive negative impulse current, optimize electroplating tank structure and change current density etc.
Fill in traditional hole is to adopt the method for determining electric current, but there is multiple situation in the current density during with the method electro-coppering at the bottom of current density and the hole in aperture, because a current value has multiple magnitudes of voltage corresponding with it on electrochemistry curve, if phenomenon is sealed in the easy generation of current density that the current density in aperture is greater than at the bottom of hole in advance, fill the silicon through hole that especially depth-to-width ratio is larger even if add multiple organic additive also cannot realize good hole in plating solution.
Therefore, although current method makes great progress in Optimization of Copper filling problem, but still exist some urgently to need the problem solving for how thoroughly solving defect in hole, so a kind of research and develop new plating filling method seems particularly necessary.
Summary of the invention
The above-mentioned shortcoming existing for prior art, the invention provides a kind of copper-connection and electroplate fill method, the present invention is simple to operation, not only more effectively control the CURRENT DISTRIBUTION in copper-connection raceway groove and through hole, the depositing current density of raceway groove or via bottoms is maximized, the current density minimum on aperture and surface, finally realize various raceway grooves, the superfill of through hole, and along with the carrying out of filling, although the geometry of raceway groove and through hole can great changes will take place, but because being adopts to determine control of Electric potentials, can make the sedimentation rate in aperture remain minimum, finally realize flawless perfect filling.
The present invention is achieved by the following technical solutions, the present invention relates to a kind of copper-connection and electroplate fill method, comprises the following steps:
Step (1), using the copper plating bath of filling for hole as electrolyte, is put into three-electrode system, measures its electrochemistry curve;
Step (2) is determined current peak and magnitude of voltage corresponding to electric current paddy difference according to electrochemistry curve;
Step (3) is put into three-electrode system using the sample with pore structure as working electrode, its electrolyte is identical with the electrolyte in step (1), then applies voltage, makes the voltage of hole surface corresponding to voltage corresponding to electric current paddy on electrochemistry curve, after energising, sample is taken out;
The thickness of copper is filled in step (4) measured hole cross section everywhere, and its thickness is corresponding to the position of current peak on electrochemistry curve;
Step (5) is adjusted the concentration of copper plating bath, change the position of current peak and electric current paddy on its electrochemistry curve, make the voltage of hole surface in electro-coppering process corresponding to voltage corresponding to electric current paddy on electrochemistry curve, voltage at the bottom of hole is corresponding to voltage corresponding to current peak on electrochemistry curve, just can produce " bottom-up " filling forms, realize flawless hole and fill.
Preferably, described copper plating bath of filling for hole comprises the copper ion that concentration is 0～100mol/L, chlorion, accelerator, inhibitor and the leveling agent that concentration is 0～1000ppm, and pH value is 1～7. Preferred, described accelerator is sodium polydithio-dipropyl sulfonate (SPS) or 3-sulfydryl propane sulfonic acid; Described inhibitor is polyethylene glycol (PEG) or polypropylene glycol; Described leveling agent is polyalkyleneimine, alkyl imidazoline, auramine or janus green B(JGB).
Preferably, described three-electrode system is made up of working electrode, auxiliary electrode and reference electrode, and described working electrode is noble metal electrode; Described auxiliary electrode is inert electrode; Described reference electrode is saturated calomel electrode, silver/silver chloride electrode or mercury/mercuric oxide electrode. Preferred, described noble metal electrode is gold, silver or platinum, and described inert electrode is gold or platinum.
Preferably, described electrochemistry curve, refers to current-voltage curve; Preferred, described current-voltage curve is cyclic voltammetric (CV) curve or linear sweep voltammetry (LSV) curve.
The sample preferably, with pore structure is the sample that surface forms hole or groove after treatment.
Compared with prior art, beneficial effect of the present invention is as follows:
The inventive method, according to the feature polarization curve of copper facing filling electrolyte electrochemical cathode, adopts special three-electrode system to carry out determining current potential electro-deposition copper facing. Method of determining current potential electro-coppering of the present invention can directly make the current density at the bottom of the current density in aperture is less than hole, and keep the current density at the bottom of the current density in aperture is less than hole in the process of filler opening always, finally realize good " bottom-up " filler opening form. The present invention not only more effectively controls the CURRENT DISTRIBUTION in copper-connection raceway groove and through hole, the depositing current density of raceway groove or via bottoms is maximized, the current density minimum on aperture and surface, finally realize the superfill of various raceway grooves, through hole, and along with the carrying out of filling, although the geometry of raceway groove and through hole can great changes will take place, because being adopts to determine control of Electric potentials, can make the sedimentation rate in aperture remain minimum, finally realize flawless perfect filling. The present invention is simple to operation, can be widely used in the high-end electronic manufacturing fields such as the copper facing filling of chip copper-connection raceway groove, 3-D stacks chip silicon through hole and high-density packages substrate through-hole.
Brief description of the drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is 0.3mol/LCu2+、50ppmCl-, 4ppmSPS, 300ppmPEG, 100ppmJGB, the pH value plating solution that is 1 LSV curve and determine the schematic diagram that current potential is electroplated.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail. Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention. It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement. These all belong to protection scope of the present invention.
Embodiment 1
The present embodiment relates to a kind of copper-connection and electroplates fill method, and concrete steps are as follows:
The copper plating bath that step (1) is filled for hole consists of the copper ion of 0.3mol/L, concentration is the chlorion of 50ppm, 4ppmSPS, 300ppmPEG, 100ppmJGB, pH value are 1, using this plating solution as electrolyte, gold plaque is working electrode, and platinized platinum is auxiliary electrode, and saturated calomel electrode is reference electrode, measure its linear sweep voltammetry (LSV) curve, as shown in Figure 1;
Step (2) is determined current peak and magnitude of voltage corresponding to electric current paddy difference according to LSV curve;
Step (3) is using the silicon chip with pore structure as working electrode, copper sheet is to electrode, saturated calomel electrode is reference electrode, be placed in the electrolytic copper plating solution identical with step (1), apply voltage, make the voltage of silicon through-hole surfaces corresponding to voltage corresponding to electric current paddy on electrochemistry curve, energising a period of time after after, by silicon chip extracting;
The thickness of copper is filled in step (4) measured hole cross section everywhere, and its thickness is corresponding to the position of current peak on electrochemistry curve;
Step (5) is adjusted the concentration of copper plating bath, change the position of current peak and electric current paddy on its electrochemistry curve, make the voltage of hole surface in electro-coppering process corresponding to voltage corresponding to electric current paddy on electrochemistry curve, voltage at the bottom of hole is corresponding to voltage corresponding to current peak on electrochemistry curve, just can produce " bottom-up " filling forms, realize flawless hole and fill.
Embodiment 2
The present embodiment relates to a kind of copper-connection and electroplates fill method, and concrete steps are as follows:
The copper plating bath that step (1) is filled for hole consists of the copper ion of 0.3mol/L, concentration is the chlorion of 50ppm, 4ppmSPS, 300ppmPEG, 100ppmJGB, pH value are 1, using this plating solution as electrolyte, silver strip is working electrode, and gold plaque is auxiliary electrode, and silver/silver chloride electrode is reference electrode, measure its linear sweep voltammetry (LSV) curve, as shown in Figure 1; Step (2) is determined current peak and magnitude of voltage corresponding to electric current paddy difference according to LSV curve;
Step (3) is using the silicon chip with pore structure as working electrode, copper sheet is to electrode, saturated calomel electrode is reference electrode, be placed in the electrolytic copper plating solution identical with step (1), apply voltage, make the voltage of silicon through-hole surfaces corresponding to voltage corresponding to electric current paddy on electrochemistry curve, energising a period of time after after, by silicon chip extracting;
The thickness of copper is filled in step (4) measured hole cross section everywhere, and its thickness is corresponding to the position of current peak on electrochemistry curve;
Step (5) is adjusted the concentration of copper plating bath, change the position of current peak and electric current paddy on its electrochemistry curve, make the voltage of hole surface in electro-coppering process corresponding to voltage corresponding to electric current paddy on electrochemistry curve, voltage at the bottom of hole is corresponding to voltage corresponding to current peak on electrochemistry curve, just can produce " bottom-up " filling forms, realize flawless hole and fill.
Embodiment 3
The present embodiment relates to a kind of copper-connection and electroplates fill method, and concrete steps are as follows:
The copper plating bath that step (1) is filled for hole consists of the copper ion of 0.3mol/L, concentration is the chlorion of 50ppm, 4ppmSPS, 300ppmPEG, 100ppmJGB, pH value are 1, using this plating solution as electrolyte, platinized platinum is working electrode, and gold plaque is auxiliary electrode, and mercury/mercuric oxide electrode is reference electrode, measure its linear sweep voltammetry (LSV) curve, as shown in Figure 1;
Step (2) is determined current peak and magnitude of voltage corresponding to electric current paddy difference according to LSV curve;
Step (3) is using the silicon chip with pore structure as working electrode, copper sheet is to electrode, saturated calomel electrode is reference electrode, be placed in the electrolytic copper plating solution identical with step (1), apply voltage, make the voltage of silicon through-hole surfaces corresponding to voltage corresponding to electric current paddy on electrochemistry curve, energising a period of time after after, by silicon chip extracting;
The thickness of copper is filled in step (4) measured hole cross section everywhere, and its thickness is corresponding to the position of current peak on electrochemistry curve;
Step (5) is adjusted the concentration of copper plating bath, change the position of current peak and electric current paddy on its electrochemistry curve, make the voltage of hole surface in electro-coppering process corresponding to voltage corresponding to electric current paddy on electrochemistry curve, voltage at the bottom of hole is corresponding to voltage corresponding to current peak on electrochemistry curve, just can produce " bottom-up " filling forms, realize flawless hole and fill.
Implementation result
Fig. 1 has shown that identical pore structure electroplates the schematic diagram of electroplating under same potential from different pore structures under different potentials, the voltage of hole surface equals voltage corresponding to electric current paddy on electrochemistry curve, if now the voltage of hole bottom is between voltage corresponding to current peak and voltage corresponding to electric current paddy, can realize " bottom-up " fills, so-called " bottom-up " filling forms refers to, in the time that copper deposits, the copper sedimentation rate of bottom, hole is greater than the copper sedimentation rate in aperture. Marker I in Fig. 1 be at the bottom of hole voltage just in time corresponding to voltage corresponding to current peak, current density at the bottom of hole is greater than the current density in aperture in this case, and because aperture place voltage is fixed, in the process of filler opening, although the shape in hole constantly changes, but the voltage at the bottom of hole between voltage corresponding to current peak and voltage corresponding to electric current paddy, so the current density at the bottom of hole is greater than the current density in aperture always, is finally realized flawless filling always. So-called current peak and electric current paddy, refer to due to the interaction between additive, a current peak and an electric current paddy on electrochemistry curve, are there is, before current peak occurs, be mainly the absorption of accelerator, between current peak and electric current paddy, be the process that inhibitor replaces accelerator absorption, after electric current paddy, reached the equilibrium stage of accelerator absorption and inhibitor absorption.
If the voltage in aperture equals the voltage that electric current paddy is corresponding, and because hole depth is larger, make voltage corresponding to current peak in hole wall somewhere, as shown in the marker II in Fig. 1, it is maximum that this place's copper sedimentation rate reaches, and will produce cavity like this between at the bottom of this place and hole. Solution is exactly that the proportioning of adjusting additive in plating solution expands the potential difference between current peak and electric current paddy, makes voltage at the bottom of hole between voltage corresponding to current peak and voltage corresponding to electric current paddy.
If the voltage in aperture is not in the voltage place that electric current paddy is corresponding, as shown in the marker III in Fig. 1, IV, V, all cannot realize the good superfill in hole, so the present invention propose determine potentiometry and can effectively realize good hole and fill.
Above specific embodiments of the invention are described. It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. copper-connection is electroplated a fill method, it is characterized in that, comprises the following steps:
Step (1), using the copper plating bath of filling for hole as electrolyte, is put into three-electrode system, measures its electrochemistryCurve;
Step (2) is determined current peak and magnitude of voltage corresponding to electric current paddy difference according to electrochemistry curve;
Step (3) is put into three-electrode system using the sample with pore structure as working electrode, its electrolyte and step(1) electrolyte in is identical, then applies voltage, makes the voltage of hole surface corresponding to electric current paddy pair on electrochemistry curveThe voltage of answering, after energising, takes out sample;
The thickness of copper is filled in step (4) measured hole cross section everywhere, and its thickness is corresponding to current peak on electrochemistry curvePosition;
Step (5) is adjusted the concentration of copper plating bath, changes the position of current peak and electric current paddy on its electrochemistry curve, makes at electricityIn copper facing process, the voltage of hole surface is corresponding to voltage corresponding to electric current paddy on electrochemistry curve, and the voltage at the bottom of hole is corresponding to electricityVoltage corresponding to current peak on chemistry curve, just can produce " bottom-up " filling forms, realizes flawless hole and fills outFill.
2. copper-connection according to claim 1 is electroplated fill method, it is characterized in that, described plating of filling for holeCopper liquid comprises copper ion that concentration is 0.3～100mol/L, chlorion, accelerator that concentration is 50～1000ppm, presses downPreparation and leveling agent, pH value is 1.
3. copper-connection according to claim 2 is electroplated fill method, it is characterized in that, described accelerator is poly-two sulphurTwo propane sulfonic acid sodium or 3-sulfydryl propane sulfonic acid.
4. copper-connection according to claim 2 is electroplated fill method, it is characterized in that, described inhibitor is poly-second twoAlcohol or polypropylene glycol.
5. copper-connection according to claim 2 is electroplated fill method, it is characterized in that, described leveling agent is poly-alkyleneBase imines, alkyl imidazoline, auramine or janus green B.
6. copper-connection according to claim 1 is electroplated fill method, it is characterized in that, described three-electrode system is by workMake electrode, auxiliary electrode and reference electrode composition, described working electrode is noble metal electrode; Described auxiliary electrode is inertiaElectrode; Described reference electrode is saturated calomel electrode, silver/silver chloride electrode or mercury/mercuric oxide electrode.
7. copper-connection according to claim 6 is electroplated fill method, it is characterized in that, described noble metal electrode be golden,Silver or platinum, described inert electrode is gold or platinum.
8. copper-connection according to claim 1 is electroplated fill method, it is characterized in that, described electrochemistry curve is electricityStream-voltage curve.
9. copper-connection according to claim 8 is electroplated fill method, it is characterized in that, described current-voltage curve isCyclic voltammetry curve or linear sweep voltammetry curve.
10. copper-connection according to claim 1 is electroplated fill method, it is characterized in that, described in there is the sample of pore structureProduct are the sample that surface forms hole or groove after treatment.
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| CN105451455A (en) * | 2014-08-06 | 2016-03-30 | 上海量子绘景电子股份有限公司 | Method for preparing fine line circuit board by filling grooves by means of selective plating |
| CN105543907A (en) * | 2015-12-09 | 2016-05-04 | 深圳市正天伟科技有限公司 | High-current-density-resistant copper electroplating additive and preparation method thereof |
| CN111081869B (en) * | 2019-10-18 | 2021-09-28 | 华中科技大学 | Method for integrating phase change memory cell by using electrochemical deposition |
| CN110911555B (en) * | 2019-10-18 | 2021-10-01 | 华中科技大学 | Deep hole superlattice filling method based on electrochemical deposition |
| CN110983389B (en) * | 2019-12-31 | 2020-11-13 | 广州三孚新材料科技股份有限公司 | Cyanide-free alkaline copper electroplating solution for steel parts and preparation method thereof |
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| US10256142B2 (en) * | 2009-08-04 | 2019-04-09 | Novellus Systems, Inc. | Tungsten feature fill with nucleation inhibition |
| US8956973B2 (en) * | 2012-03-27 | 2015-02-17 | International Business Machines Corporation | Bottom-up plating of through-substrate vias |
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