CN108169313B - Characterization and calibration method and device for TSV electroplating additive parameters - Google Patents
Characterization and calibration method and device for TSV electroplating additive parameters Download PDFInfo
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Abstract
The invention relates to an electroplating solution exchange current density
And cathode transfer coefficient
The invention also provides a characterization and calibration method of the diffusion coefficient of the TSV electroplating additive, which is used for testing by a chronoamperometry method.
Description
Technical Field
The invention relates to the field of electrochemistry, in particular to a characterization and calibration method for TSV electroplating additive parameters.
Background
Integrated Circuit (IC) technology is rapidly developed according to moore's law, high-density circuit integration requires high-density interconnection technology, and in order to improve device performance and interconnection density, a three-dimensional integrated package technology with Through Silicon Via (TSV) interconnection as a core is a necessary trend in development. The TSV technology is a method for directly penetrating through a silicon wafer to realize vertical up-down interconnection among stacked chips and form a high-density three-dimensional integrated chip, and has the advantages of high density, multiple functions, small size and the like.
The diameter of the TSV hole is usually tens of microns, the aspect ratio can be as high as 10-20, and copper is usually used as a filler. In the field of three-dimensional integrated packaging of integrated circuits, high aspect ratio through-silicon via filling is an important technical challenge. Among them, the addition of various additives (suppressor, accelerator and leveler) to the plating solution to improve the TSV filling process and thereby achieve defect-free filling is a common method in the industry. In the TSV electro-coppering technique, various parameters are difficult to determine due to the complexity of the mechanism of action of the additive in the bath. Therefore, the invention provides a novel method for rapidly and accurately characterizing and calibrating various additive parameters (such as exchange current density, cathode transfer coefficient and diffusion coefficient of the additive) in TSV electroplating.
Disclosure of Invention
Exchange current density (i)0) And cathode transfer coefficient (α)c) The characterization and calibration method adopts linear sweep voltammetry, and is based on the following system which comprises the following steps: a computer, an electrochemical workstation, a working electrode, a reference electrode, a counter electrode, a test solution and an electroplating bath;
a working electrode: the reaction of converting copper ions into copper takes place at this electrode. The working electrode is typically composed of an inert metal. It is usually a rotating disk electrode that is used to study the chemical reaction mechanism of the test solution. In this experiment, the working electrode was a platinum rotating disk electrode;
counter electrode: the current flowing through the working electrode flows entirely through this electrode. In this experiment, the counter electrode was a platinum electrode;
reference electrode: the electrode maintains a stable and known electrode voltage. The reference electrode is used as a reference for measuring and controlling the voltage of the working electrode. In this experiment, the reference electrode was a mercurous sulfate electrode;
the positive pole of the power supply in the electrochemical workstation is connected with a counter electrode (electroplating anode), the negative pole is connected with a working electrode and a reference electrode (electroplating cathode), and the electrodes are all immersed in electroplating solution in an electroplating bath;
the electrochemical workstation is controlled by a computer;
exchange current density (i)0) And cathode transfer coefficient (α)c) The characterization and calibration method comprises three processes of experiment preparation, linear sweep voltammetry test and result calculation;
the experimental preparation process comprises the following steps:
step 1: preparing a test solution;
step 2: polishing and cleaning the electrode;
and step 3: injecting a test solution and installing an electrode;
and 4, step 4: connecting a lead connected with the chemical workstation;
the linear sweep voltammetry test procedure included the following steps:
step 1: linear sweep voltammetry testing;
step 2: cleaning an electrode;
the result calculation process includes the following steps:
step 1: drawing lni-V curve graphs and applying the formula (1) to calculate;
wherein i is the measured plating current density, n is the copper ion valence, F is the Faraday constant, R is the gas constant, T is the temperature, V is the plating overpotential, i is the plating overpotential0Desired exchange Current Density for the experiments, αcThe electron transfer coefficient of the cathode is desired for the experiment.
The invention also provides a characterization and calibration method of the diffusion coefficient of the TSV electroplating additive, a Chronoamperometry (CA) method is adopted, and the system comprises the following systems: a computer, an electrochemical workstation, a working electrode, a reference electrode, a counter electrode, a test solution, an additive, an injection hole and an electroplating bath;
the positive pole of the power supply in the electrochemical workstation is connected with a counter electrode (electroplating anode), the negative pole is connected with a working electrode and a reference electrode (electroplating cathode), and the electrodes are all immersed in electroplating solution in an electroplating bath;
the electrochemical workstation is controlled by a computer;
the characterization and calibration method of the diffusion coefficient of the additive comprises three processes of experiment preparation, Chronoamperometry (CA) test and result calculation;
the experimental preparation process comprises the following steps:
step 1: preparing a test solution;
step 2: polishing and cleaning the electrode;
and step 3: mounting a test solution and an electrode;
and 4, step 4: connecting a lead connected with the chemical workstation;
the chronoamperometry testing procedure comprises the steps of:
step 1: testing by a chronoamperometry method;
step 2: cleaning an electrode;
the result calculation process includes the following steps:
step 1: calculating the diffusion coefficient by applying the formula (2);
where τ is the time constant, i.e., the time required for the additive to diffuse to the working electrode after injection, δ is the thickness of the Nernst diffusion boundary layer obtained by the Levich equation, DAddThe diffusion coefficient of the additive that is desired to be obtained for the experiment.
The invention has the beneficial effects that:
in the TSV copper electroplating technology, due to the complexity of the action mechanism of the additive in the electroplating solution, various parameters are difficult to determine, and the method utilizes an electrochemical workstation and designs a simple test method, so that the exchange current density, the cathode transfer coefficient and the additive diffusion coefficient of the electroplating solution can be conveniently and effectively obtained.
Drawings
FIG. 1 is a system of a device for linear sweep voltammetry;
FIG. 2 is a rotary disk electrode system;
FIG. 3 is a three electrode system;
FIG. 4 is the lni-V curve of example 1;
FIG. 5 is a chronoamperometry testing apparatus;
FIG. 6 illustrates electrode placement and additive injection;
FIG. 7 is a graph of the change in current density with time resulting from the addition of the inhibitor in example 2;
FIG. 8 is a graph of the change in current density with time resulting from the addition of an accelerator in example 3;
FIG. 9 is a graph of the current density as a function of time resulting from the addition of a leveler in example 4;
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and the accompanying drawings.
Example 1:
the exchange current density and cathodic transfer coefficient of the plating bath without TSV plating additive were measured by linear voltammetry. Linear sweep voltammetry measures the current of the working electrode, where the voltage between the working electrode and the reference electrode varies linearly with time.
Exchange current density: when the electrode reactions are in equilibrium, the rates of progress of the electrode reactions in both directions are equal, and the absolute values of the current densities of the anode reaction and the cathode reaction, which proceed in both reaction directions, are called exchange current densities.
Cathode transfer coefficient: the extent of increase in the active gibbs free energy of the cathodic reduction reaction is characterized.
The first step is as follows: preparation of test solutions
Measuring 40 ml of SYS2510 electroplating solution as a test solution by using a beaker;
the second step is that: electrode pretreatment
Polishing the electrode by using abrasive paper to remove an oxide layer on the surface of the electrode, and cleaning the polished electrode by using deionized water to ensure good conductivity of the electrode;
the third step: test solution was injected into the plating bath and electrodes were installed
The prepared test solution was poured into an electroplating bath, and a counter electrode (platinum electrode), a working electrode (platinum rotating disk electrode) and a reference electrode (mercurous sulfate electrode) were mounted on the experimental apparatus as shown in fig. 2;
the fourth step: connecting a conductor to a chemical workstation
Connecting a serial port connected to a computer on an electrochemical workstation with the computer as shown in FIG. 1, and respectively connecting connectors of three electrodes on the electrochemical workstation with a counter electrode, a working electrode and a reference electrode;
the fifth step: performing a test of Linear voltammetric Scan
Starting an electroplating power supply on an electrochemical workstation to enable copper ions to be converted into copper on a cathode, setting the scanning rate of the voltage between a working electrode and a reference electrode along with the change of time to be 2mV/s on a computer, and measuring and recording the current passing through the working electrode;
and a sixth step: cleaning electrode
After the electroplating is finished, taking the counter electrode, the working electrode and the reference electrode out of the electroplating solution, washing the electrodes by deionized water, and collecting for the next use;
the seventh step: calculation results
The lni-V plot was plotted from the recorded voltage applied to the working electrode and the current through the working electrode, as shown in FIG. 4, analyzed and fitted to i by the Butler-Volmer equation0And αcAs shown in equation (1).
The lni-V graph shows three regions, as shown in FIG. 4, namely: the I area is a Tafel area, the II area is a transition area, and the III area is a limiting current area. Fitting the curve of the first region to obtain a fitting equation of which y is kx + b, and substituting the formula (1) into the fitting equation to obtain the exchange current density i0And a cathode transfer coefficient αc。
The current flowing through the electrode as a function of time was recorded by applying a certain voltage to the working electrode by Chronoamperometry (CA). By testing the time-varying current flowing through the working electrode at a set applied voltage, a corresponding electrochemical analysis can be performed
The characterization and calibration method comprises the following steps: the time constant (τ) is obtained by chronoamperometry, and the diffusion coefficient is then calculated using the scaled transient diffusion equation (i.e., equation (2)), where the thickness of the Nemst diffusion boundary layer (6) can be obtained by the Levich equation
Example 2:
characterization and calibration of diffusion coefficients of inhibitors in electroplating baths
The first step is as follows: preparation of test solutions
Measuring 35 ml of SYS2510 solution as electroplating solution, placing into a beaker, and using a syringe to obtain 5 ml of mixed solution containing 4.6 ml of SYS2510 and 0.4 ml of UPT3320S as additives;
the second step is that: electrode pretreatment
Polishing the electrode by using abrasive paper to remove an oxide layer on the surface of the electrode, and cleaning the polished electrode by using deionized water to ensure good conductivity of the electrode;
the third step: test solution was injected into the plating bath and electrodes were installed
Injecting 35 ml of SYS2510 solution prepared in a beaker into an electroplating bath, and installing a counter electrode (platinum electrode), a working electrode (platinum rotating disc electrode) and a reference electrode (mercurous sulfate electrode) on an experimental device according to the structure shown in FIG. 5;
the fourth step: connecting a conductor to a chemical workstation
Connecting a serial port connected to a computer on the electrochemical workstation with the computer according to the diagram shown in FIG. 2, and connecting connectors of three electrodes on the electrochemical workstation with a counter electrode, a working electrode and a reference electrode respectively according to the diagram shown in FIG. 5;
the fifth step: performing a Chronoamperometric (CA) test
Starting an electroplating power supply on an electrochemical workstation to enable a reaction of converting copper ions into copper to occur on a cathode, applying a voltage of-0.6V to a working electrode on a computer, setting the rotation speed of an electroplating solution stirrer to be 600rpm, injecting 5 ml of mixed solution containing an inhibitor into the electroplating solution from an injection hole by using an injector shown in figure 6 at the time of 50 seconds, cutting off the power supply after 200 seconds (until a steady state is reached), stopping the experiment, measuring and recording the current passing through the working electrode in the experiment process;
and a sixth step: cleaning electrode
After the electroplating is finished, taking the counter electrode, the working electrode and the reference electrode out of the electroplating solution, washing the electrodes by deionized water, and collecting for the next use;
the seventh step: calculation results
The i-t plot is plotted against the recorded current through the working electrode, as shown in fig. 7, and the diffusion coefficient is analyzed and calculated by scaling the transient diffusion equation, as shown in equation (2).
The time-current density plot shows four phases, namely: the stage I is a plating solution non-steady state stage, the stage II is a plating solution steady state stage, the stage III is an inhibitor diffusion stage, and the stage IV is a mixed solution steady state stage. The time constant is the time for the inhibitor to diffuse to the working electrode. The diffusion coefficient of the suppressor in the plating liquid is calculated using the formula (2).
Example 3:
characterization and calibration of accelerator diffusion coefficient in electroplating baths
The first step is as follows: preparation of test solutions
Measuring 4.875 ml of SYS2510 and 34.125 ml of deionized water, mixing to obtain a plating solution, placing the plating solution in a beaker, and using a syringe to obtain 1 ml of UPT3320A solution as an additive;
the second step is that: electrode pretreatment
Polishing the electrode by using abrasive paper to remove an oxide layer on the surface of the electrode, and cleaning the polished electrode by using deionized water to ensure good conductivity of the electrode;
the third step: test solution was injected into the plating bath and electrodes were installed
4.875 ml of SYS2510 and 34.125 ml of deionized water prepared in a beaker were poured into an electroplating bath, and a counter electrode (platinum electrode), a working electrode (platinum rotating disk electrode) and a reference electrode (saturated calomel electrode) were mounted on an experimental apparatus as shown in FIG. 5;
the fourth step: connecting a conductor to a chemical workstation
Connecting a serial port connected to a computer on an electrochemical workstation with the computer as shown in FIG. 1, and respectively connecting connectors of three electrodes on the electrochemical workstation with a counter electrode, a working electrode and a reference electrode;
the fifth step: performing a Chronoamperometric (CA) test
Starting an electroplating power supply on an electrochemical workstation to enable a reaction of converting copper ions into copper to occur on a cathode, applying a voltage of-0.6V on a working electrode on a computer, setting the rotation speed of an electroplating solution stirrer to be 600rpm, injecting 1 ml of UPT3320A solution into the electroplating solution from an injection hole by using an injector at the time of 50 seconds, cutting off the power supply after 200 seconds (until a steady state is reached), stopping the experiment, and measuring and recording the current passing through the working electrode in the experiment process;
and a sixth step: cleaning electrode
After the electroplating is finished, taking the counter electrode, the working electrode and the reference electrode out of the electroplating solution, washing the electrodes by deionized water, and collecting for the next use;
the seventh step: calculation results
The i-t plot is plotted against the recorded current through the working electrode, as shown in fig. 8, and the diffusion coefficient is analyzed and calculated by scaling the transient diffusion equation, as shown in equation (2).
The time-current density plot shows six phases, namely: the first stage is the unstable stage of the electroplating solution, the second stage is the stable stage of the electroplating solution, the third stage is the diffusion stage of the accelerator, the fourth stage is the consumption stage of copper ions in the diffusion layer, the fifth stage is the unstable stage of the mixed solution, and the VI stage is the stable stage of the mixed solution. The time constant is the time for the accelerator to diffuse to the working electrode. The diffusion coefficient of the accelerator in the plating liquid is calculated using the formula (2).
Example 4:
characterization and calibration of leveler diffusion coefficients in electroplating baths
The first step is as follows: preparation of test solutions
Measuring 4.875 ml of SYS2510 and 34.125 ml of deionized water, mixing to obtain a plating solution, placing the plating solution in a beaker, and using a syringe to obtain 1 ml of UPT3320L solution as an additive;
the second step is that: electrode pretreatment
Polishing the electrode by using abrasive paper to remove an oxide layer on the surface of the electrode, and cleaning the polished electrode by using deionized water to ensure good conductivity of the electrode;
the third step: test solution was injected into the plating bath and electrodes were installed
4.875 ml of SYS2510 and 34.125 ml of deionized water prepared in a beaker were poured into an electroplating bath, and a counter electrode (platinum electrode), a working electrode (platinum rotating disk electrode) and a reference electrode (saturated calomel electrode) were mounted on an experimental apparatus as shown in FIG. 5;
the fourth step: connecting a conductor to a chemical workstation
Connecting a serial port connected to a computer on an electrochemical workstation with the computer as shown in FIG. 1, and respectively connecting connectors of three electrodes on the electrochemical workstation with a counter electrode, a working electrode and a reference electrode;
the fifth step: performing a Chronoamperometric (CA) test
Starting an electroplating power supply on an electrochemical workstation to enable a reaction of converting copper ions into copper to occur on a cathode, applying a voltage of-0.6V on a working electrode on a computer, setting the rotation speed of an electroplating solution stirrer to be 600rpm, injecting 1 ml of UPT3320L solution into the electroplating solution from an injection hole by using an injector at the time of 50 seconds, cutting off the power supply after 200 seconds (until a steady state is reached), stopping the experiment, and measuring and recording the current passing through the working electrode in the experiment process;
and a sixth step: cleaning electrode
After the electroplating is finished, taking the counter electrode, the working electrode and the reference electrode out of the electroplating solution, washing the electrodes by deionized water, and collecting for the next use;
the seventh step: calculation results
The i-t plot is plotted against the recorded current through the working electrode, as shown in fig. 9, and the diffusion coefficient is analyzed and calculated by scaling the transient diffusion equation, as shown in equation (2).
The time-current density plot shows five phases, namely: the first stage is an unstable stage of the electroplating solution, the second stage is a stable stage of the electroplating solution, the third stage is a leveler diffusion stage, the fourth stage is an unstable stage of the mixed solution, and the fifth stage is a stable stage of the mixed solution. The time constant is the time for the leveler to diffuse to the working electrode. The diffusion coefficient of the leveler in the plating solution is calculated using equation (2).
Wherein i is the measured plating current density, n is the copper ion valence, F is the Faraday constant, R is the gas constant, T is the temperature, V is the plating overpotential, i is the plating overpotential0Is made ofExpected exchange Current Density, αcThe electron transfer coefficient of the cathode is desired for the experiment.
Where τ is the time constant, i.e., the time required for the additive to diffuse to the working electrode after injection, δ is the thickness of the Nernst diffusion boundary layer obtained by the Levich equation, DAddThe diffusion coefficient of the additive that is desired to be obtained for the experiment.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A characterization and calibration method for diffusion coefficient of TSV electroplating additive is characterized in that a chronoamperometry method is adopted for testing, and a formula (2) is applied to calculate the diffusion coefficient DAdd：
Wherein τ is a time constant, i.e., the time required for the additive to diffuse to the working electrode after injection, the time constant is obtained by chronoamperometry, and δ is the thickness of the Nernst diffusion boundary layer obtained by the Levich equation.
2. The method of claim 1, further comprising a preparation process, the preparation process comprising the steps of:
step 1: preparing a test solution;
step 2: polishing and cleaning the electrode;
and step 3: mounting a test solution and an electrode;
and 4, step 4: the wire connected to the chemical workstation is switched on.
3. The method of claim 2, said step 1 comprising placing a plating solution in a beaker; the syringe is prepared for mixing solutions including the plating solution and the additive to be tested.
4. The method of claim 3, wherein the power supply for the electroplating at the electrochemical station is turned on to allow the reaction of converting copper ions into copper to occur at the cathode, the applied voltage is 0.1 to 1V in the chronoamperometric test, and the mixed solution is injected 10 to 90 seconds after the power supply is turned on.
5. The method of claim 4, wherein the chronoamperometric assay is performed at a voltage of 0.5 to 0.8V and the mixed solution is injected 30 to 70 seconds after the power is turned on.
6. The method of claim 4, wherein the mixed solution is injected 40-60 seconds after power-on, and the electrode is cleaned after the test.
7. The method of claim 1, the additive comprising one of an inhibitor, an accelerator, and a leveler.
8. A system for testing according to the method of claim 1, comprising: a computer, an electrochemical workstation, a working electrode, a reference electrode, a counter electrode, a test solution, an additive, an injection hole and an electroplating bath.
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