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In-situ real-time ellipsometric investigations during the atomic layer deposition of ruthenium: A process development from [(ethylcyclopentadienyl)(pyrrolyl)ruthenium] and molecular oxygen
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10.1116/1.3670405
/content/avs/journal/jvsta/30/1/10.1116/1.3670405
http://aip.metastore.ingenta.com/content/avs/journal/jvsta/30/1/10.1116/1.3670405

Figures

Image of FIG. 1.
FIG. 1.

(Color online) Gas pulsing sequence and the course of the controlled total process pressure (solid line) during one complete ALD cycle (55 s).

Image of FIG. 2.
FIG. 2.

High-resolution transmission electron microscopy cross-section of a (10.7 ± 0.6) nm thick and 0.87 nm rms-rough Ru ALD film indicating an underlying silicon silicon dioxide interface that was supposed to be formed during the ALD growth initiation. The thickness and roughness of the optical Ru layer stack model constituted in Table I as well as the nominal Ru film thickness calculated from Eq. (1) are illustrated aside.

Image of FIG. 3.
FIG. 3.

(Color online) Distribution of the GPC data points which interpolated the slope of the nominal Ru film thickness over ten ALD cycles under standard process conditions listed in Table II. The line represents an appropriate fitted GAUSSIAN normal distribution.

Image of FIG. 4.
FIG. 4.

(Color online) (a) Optical thicknesses of the Ru layer and the EMA layer (i.e., the surface roughness) fitted on the basis of the optical model in Table I as well as the mean squared error of the regression analysis in the course of ALD cycles. (b) The growth per cycle, interpolating the slope of the nominal Ru film thickness over ten cycles, in the progress of ALD cycles. A fairly stable growth region with negligible statistical spread resulted between 100 and 230 ALD cycles.

Image of FIG. 5.
FIG. 5.

(Color online) Growth per cycle for varying ECPR pulsing times. Each dot represents the interpolated slope of the nominal Ru film thickness over ten ALD cycles in which a respective ECPR pulsing time was set. The solid line shows the kinetic growth model of Eq. (2) fitted to the individual data points.

Image of FIG. 6.
FIG. 6.

(Color online) Growth per cycle for varying O2 pulsing times. Each dot represents the interpolated slope of the nominal Ru film thickness over ten ALD cycles in which a respective O2 pulsing time was set. The advanced kinetic growth model of Eq. (3) (solid line) relates these individual data points to each other. The dashed line represents the first growth process without superposition of the second.

Image of FIG. 7.
FIG. 7.

(Color online) Growth per cycle as a function of the Ar purging times after ECPR and O2 pulses.

Image of FIG. 8.
FIG. 8.

(Color online) Growth per cycle as a function of the real substrate temperature. Each dot represents the interpolated slope of the nominal Ru film thickness over ten ALD cycles in which a respective stabilized substrate temperature was set. The solid line serves a guide to the eye, relating the individual data points to each other.

Image of FIG. 9.
FIG. 9.

(Color online) Growth per cycle for a varied total working pressure, which was controlled to a fairly constant value employing a Baratron pressure gauge in combination with a butterfly valve.

Image of FIG. 10.
FIG. 10.

Scanning electron microscopy pictures: (a) Delamination of a 25 nm thick Ru film. (b) Improved adhesion of a comparable film produced with an intermediate annealing step after 5 nm.

Image of FIG. 11.
FIG. 11.

(Color online) Microsection of through silicon via structures with an aspect ratio of 10:1 after the direct electrochemical deposition of copper on an ALD Ru seed layer.

Tables

Generic image for table
TABLE I.

This optical layer stack model translates the ellipsometric spectra into structural film dimensions.

Generic image for table
TABLE II.

Overview of our process parameters for the thermal-activated ALD of Ru from ECPR and O2, revealed from a process development in the linear homogeneous Ru-on-Ru film growth regime.

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/content/avs/journal/jvsta/30/1/10.1116/1.3670405
2011-12-15
2014-04-21
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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: In-situ real-time ellipsometric investigations during the atomic layer deposition of ruthenium: A process development from [(ethylcyclopentadienyl)(pyrrolyl)ruthenium] and molecular oxygen
http://aip.metastore.ingenta.com/content/avs/journal/jvsta/30/1/10.1116/1.3670405
10.1116/1.3670405
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