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NIST SPECIAL PUBLICATION 400-101

U.S. DEPARTMENT OF COMMERCE/Technology Administration

National Institute of Standards and Technology

Semiconductor Measurement Technology:

Workshop on Mass Flow Measurement

and Control for the Semiconductor Industry

Robert F. Berg, David S. Green, and George E. Mattingly

IV II

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NTENNIAL*
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NIST Special Publication 400-101

Semiconductor Measurement Technology:

Workshop on Mass Flow Measurement

and Control for the Semiconductor Industry

Robert F. Berg, David S. Green, and George E. Mattingly

Chemical Science and Technology Laboratory

Process Measurements Division

National Institute of Standards and Technology

Gaithersburg, MD 20899-8360

February 2001

U.S. DEPARTMENT OF COMMERCE, Donald L Evans, Secretary

NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY, Karen H. Brown, Acting Director
Certain commercial entities, equipment, or materials may be identified in this document

in order to describe an experimental procedure or concept adequately. Such

identification is not intended to imply recommendation or endorsement by the National

Institute of Standards and Technology, nor is it intended to imply that the entities, materials, or equipment are necessarily the best available for the purpose.

National Institute of Standards and Technology Special Publication 400-101

Natl. Inst. Stand. Technol. Spec. Publ. 400-101, 89 pages (February 2001)

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Table of contents

Executive summary 1

Introduction 2

Workshop objective and format 4

Presentation abstracts

Mass flow controller performance and characterization

Gary Allen, Applied Materials 5 Gasflow standards and calibration

John Wright, NIST 6

Consistent ±3 sigma calibration

Bill Valentine, Kinetics Fluid Systems 7

The impact of various gas properties on the operation of an MFC

Dan Mudd, Mass Flow Associates of Texas 8

NIST's program to measure the thermophysical properties of

semiconductor process gases, John Hurly, NIST 8

Requirements for the next generation gas mass flow controllers

Kaveh Zarkar, Millipore 9

Discussions in the full workshop 1

1

Final recommendations 15

Appendices

A. Prioritization of the proposed tasks 17

B. Suggested topics for breakout sessions 19

C. Abbreviations and jargon 20

D. Workshop schedule 21

E. Participant addresses 22

F. Presentation viewgraphs 25

Executive summary

On 15-16 May 2000 at NIST, 45 scientists and engineers met to identify research and

standards that will benefit users and manufacturers of mass flow controllers (MFCs) and

related equipment. Most attendees represented companies closely associated with the

semiconductor industry, including manufacturers of MFCs, of process tools, and of

semiconductor devices. They were asked to:

1 . Identify the technical problems limiting the productivity of the U.S.

semiconductor manufacturing industry.

2. Prioritize the ways these problems can be resolved using NIST's assistance.

Brief presentations were given and lengthy discussions were held on the following topics:

1 . Flow meter performance.

2. Standards and calibration.

3. Gas properties.

4. Alternatives to thermal mass flow controllers.

The attendees proposed 21 tasks directed at the identified problems. A subsequent vote

identified the seven strongly recommended tasks listed below.

Strongly recommended task Institution

1 Devise a technique to verify MFC performance that is independent

of the process chamber.

none specified

2 Characterize the performance of each new MFC with nitrogen as well as with its nameplate gas. MFC

manufacturers

3 Increase the range of transfer standards for conducting round-robin

tests (0.01 seem to 1000 slm).

NIST

4 Improve the primary (0.025%) and transfer (0.1%) standards for gas

flow.

NIST

5 Expand and reprioritize the list of gases to be studied. Schedule and

conduct property measurements.

NIST

6 Establish and maintain a public, Web-based database of gas

properties.

NIST

7 Develop metrology to characterize liquid flow controllers. NIST

These recommendations will help NIST guide its research on gas properties, flow

standards, and flow measurement techniques.

1
Introduction

Flow measurements are central to the manufacture of semiconductor devices, especially

in chemical vapor deposition and plasma etch processes. A mass flow controller's

performance affects production costs in at least two ways, ^reproducibility of the MFC

increases the product's defect rate, and inaccuracy of the MFC increases the time

required to copy a process recipe from one process tool to another. As shown in the table

below, five of the technology working groups for the 1999 International Technology

Roadmap for Semiconductors raised issues related to MFC performance.

Working group Issues related to mass flow control

Design • Uncertainty due to manufacturing variability

Front end processes • Control boron penetration

• Achievement of lateral and depth abruptness

• Etch CD control and selectivity

• Sidewall etch control

Interconnect • Combinations of materials . .

.

• Low plasma damage. .

.

• As features shrink, etching and filling high aspect ratio structures will be challenging...

Factory integration • Control production equipment and factory processes to reduce parametric variation

• Minimize waste and scrap and reduce the number of

nonproduct wafers

Defect reduction • Advanced modeling (chemistry/contamination), materials

technology, software and sensors are required to provide

robust, defect-free process tools . .

.

All MFCs require both a model and a calibration. The model, which depends on the

MFC's design, relates the raw output, which might be in volts, to the final output, which

is in units of flow. The model cannot account for differences between MFCs caused by

manufacturing variations. The calibration, which is done for every MFC, accounts for

these differences.

The great variety of fluids used in semiconductor processing challenges the model. More

than 30 gases are in routine use, and the continual introduction of new processes is adding liquids as well as gases to this list. Not only must the model be sufficiently

general to accommodate different fluids, but also it must have accurate thermodynamic

and transport property data for each fluid.

The variety of fluids challenges the calibration also. Calibrations frequently use a benign

surrogate gas instead of the hazardous process gas for which the MFC is intended. With

2
the use of a surrogate gas, an error in the MFC model or in the process gas's properties

leads to an error in the calibration.

In addition to accurate property data, good models and calibrations require accurate flow

standards. An MFC model can be tested only to the accuracy of the standard, and a

calibration requires a flow standard whose accuracy exceeds that required of the MFC.

NIST has a long history of providing accurate, unbiased measurement standards and

property data. In response to the semiconductor industry, NIST recently established

programs to measure the properties of semiconductor gases and to extend gas flow

standards to lower flow rates. The workshop's recommendations will help NIST guide its research on gas properties, flow standards, and flow measurement techniques.

Acknowledgements

Gil Yetter of International Sematech introduced us to engineers concerned with flow

measurement in Austin, provided a large list of other contacts, and gave us constant

encouragement. We thank him also for the encouragement he gave to the workshop

attendees. We thank Lori Phillips Buckland of the NIST Public and Business Affairs

Division for handling many essential administrative tasks. Planning for the workshop

began under the direction of the recently retired chief of the Process Measurements

Division, Greg Rosasco. We thank him and the present division chief, James Whetstone,

for their support. Most of all, we thank the speakers, the session leaders, and the other

participants, for the time, expense, and effort they generously gave.

Funding for the workshop's planning came from the Process Measurements Division

(PMD) and the National Semiconductor Metrology Program (NSMP). The PMD

develops and provides measurement standards and services, measurement techniques,

recommended practices, sensing technology, instrumentation, and mathematical models

required for analysis, control, and optimization of industrial processes. Work supporting

flow measurements takes place in the PMD's Fluid Flow, Fluid Science, and Pressure &

Vacuum Groups. The NSMP is a NIST-wide effort designed to meet the highest priority

measurement needs of the semiconductor manufacturing industry and its supporting

industries. The National Semiconductor Metrology Program supports a broad portfolio

comprising 40 semiconductor metrology development projects at NIST.

Further information

National Institute of Standards and Technology http://www.nist.gov

Process Measurements Division http://www.cstl.nist.gov/div836/

National Semiconductor Metrology Program http://www.eeel.nist.gov/omp

Technical contacts

Robert F. Berg George E. Mattingly

100 Bureau Drive 100 Bureau Drive

NIST

Gaithersburg, MD 20899-8364

NIST

Gaithersburg, MD 20899-8360

robert.berg@nist.gov 301-975-2466 george. mattingly @nist.gov 30 1 -975-5939

3
Workshop objective and format

The objective of this two-day workshop was to identify research and standards that will

benefit users and manufacturers of mass flow controllers and related equipment The

attendees were asked to:

1 . Identify the technical problems limiting the productivity of the U.S.

semiconductor manufacturing industry.

2. Prioritize the ways these problems can be resolved using NIST's assistance.

As shown in the table below, most of the workshop attendees represented companies

closely associated with the semiconductor industry. The NIST attendees were from the

Process Measurements Division or the Office of Microelectronic Programs. Appendix E

lists the names and addresses of the attendees.

Type of institution Attendees

MFC manufacturers 1

3

semiconductor tool manufacturers 3

MFC users in semiconductor industry 4

MFC users in other industries 2

other semiconductor flow measurement companies 8

semiconductor consortia (International Sematech) 2

independent consultants 4

NIST 7

other federal laboratories (Oak Ridge National Lab) 2 TOTAL 45

Appendix D gives the workshop schedule. On the morning of the first day, brief talks set the context for the workshop's four topics:

1. Flow meter performance.

2. Standards and calibration.

3. Gas properties.

4. Alternatives to thermal mass flow controllers.

That afternoon, the attendees divided into four groups corresponding to these topics. In each group, the attendees addressed the following questions:

• What are the present requirements and how well are they realized?

• How will the requirements change over the next ten years?

• How can national laboratories such as NIST best assist industry?

On the morning of the second day, the attendees met to discuss the results from each

group. They then divided for a second, brief breakout session. That afternoon, each

breakout group presented up to six proposed tasks. Proposals presented by more than one

group were combined. The attendees then voted on the importance of the tasks.

4
Presentation abstracts

Mass flow controller performance and characterization

Gary Allen

Applied Materials

The presentation focuses on the characteristics, requirements, gases, and types of mass

flow controllers utilized currently in the semiconductor industry. The importance of flow

control in semiconductor equipment processes is paramount to the capability,

repeatability, and manufacturing of integrated circuits. MFCs (mass flow controllers) are controlled by both analog and digital connections, some digital MFCs via a standard

protocol.

The transient characteristics of gas flow into sub-atmospheric pressure chambers are important in the overall understanding of semiconductor processes. Some of these

characteristics are dead time, step response time, settling (control) time, overshoot,

repeatability and valve leak by. Other characteristics of accuracy, linearity,

reproducibility, and zero offset are also necessary in understanding the behavior of

MFCs.

In today's semiconductor industry different types of MFCs are becoming prevalent. The

most common variety in the industry are thermal-based MFCs. Pressure-based MFCs are finding applications in semiconductor processes. Two types of flow sensors which are

utilized in other industries are Coriolis and MEMS-based sensors. Although not fully

developed, these types of sensors may find semiconductor applications in the future.

Since performance requirements had not been developed for the MFCs in the

semiconductor industry, Applied Materials set forth a commodity specification to define

and test to those requirements. Utilizing a rate of rise measurement system Applied was

the first organization to characterize the transient behavior of MFC flow into a subatmospheric pressure chamber. This technique best replicates the behavior of gas

entering into a wafer process chamber.

Calibration gases, referred to as surrogate gas(s) are utilized to best replicate the

nameplate gas. The nameplate gas is the actual process gas which the MFC is calibrated

for. The relationship of surrogate to name plate gas is paramount in understanding how

to calibrate an MFC. Knowing that these relationships are non-linear, polynomial

equations can be generated to best fit the function of this relationship. Additionally the

relationships back to nitrogen, for all gases, are important so that testing of MFCs

integrated into semiconductor equipment can be tested, prior to shipment and installation

in the fab.

Performance evaluation is a necessary evil for understanding which MFCs are best for a

specific semiconductor process. The testing requirements allow for ranking of suppliers,

5
and for interactive development of MFCs with the manufacturers of these instruments.

Additionally, comparative analysis, such as: the analog vs. digital; along with thermal vs. pressure based and the like can be reviewed.

The improvements in calibrations, diagnostics, and digital communication protocols have

enhanced the capabilities of MFCs and allow for statistical process control methods to be

applied. This should allow for process repeatability improvements, necessary in the

development of semiconductor processes.

Issues which need to be overcome are: Cross-talk, pressure regulator interaction, and gas

bursting; these phenomenon and behaviors are evident in the issues which semiconductor

manufacturers face on a daily basis. Also the behavior of various types of MFCs need to be studied and understood. Are various types of MFCs affected by the same

phenomenon? Liquid and subatmospheric delivery regimes also require testing,

understanding, and evaluation in order to develop and improve semiconductor processes.

I hope that this presentation stirs interest in the terminology, issues, behavior,

performance and understanding of how MFCs are manufactured and applied in today's

semiconductor industry.

Gas flow standards and calibration

John D. Wright

National Institute of Standards and Technology

The Fluid Flow Group at the National Institute of Standards and Technology in Gaithersburg, Maryland offers calibration services for flow meters used in gas, water, and

liquid hydrocarbon. Gas flow meters are calibrated with piston provers, bell provers, or PVTt systems for flows between 0.04 L/min and 78000 L/min. Further details of these

calibration services are documented, including the principle of operation and

measurement uncertainties. The definition of traceability (direct and indirect) and the

importance of proficiency tests that include inter-laboratory comparisons are discussed.

6
Consistent ±3 sigma calibration

Bill Valentine

Kinetics Fluid Systems

MFC manufacturers have been claiming an accuracy of ±1% FS since the invention of

the MFC. Several years ago, Unit Instruments set out to create a metrology system

capable of delivering product such that 99.7% (±3 sigma) of all product shipped would

meet an accuracy of ±1% FS. Unit Instruments' strategy consisted of a three-tier attack.

First step was to understand our capabilities in metrology. We developed a system called

Crosscheck, where we compare various primary standards against each other. The

primary calibration techniques utilized in our system are constant volume (bell prover),

constant pressure (rate-of-rise) and gravimetric. These calibration methods do not share

common modes of error. Consequently, comparing primaries against each other is the

most effective method to determine if one of your calibration techniques has degraded. In addition to comparing primaries internally, we participate in round robin comparisons

with NIST. Critical flow nozzles are used to check metrology between service centers

and our main metrology center, and laminar flow elements are used to transfer metrology

to the production floor.

Next, we set out to determine if we had a capable process. 1092 MFCs were screened over a period of 14 months. The MFCs were selected to cover a wide range of gases and

ranges. Calibration was verified on two different calibration stations. The measurements

statistically demonstrated our process was capable to ± three sigma limits.

Finally, we needed to show our solid metrology and production process would translate

into superior on tool performance. Accuracy on nitrogen does not insure a MFC will

perform on tool with the process gas. Using our onsite gravimetric facility and a gravimetric facility at Oak National Laboratory, we validated our product was linear and

thus its surrogate gas calibration would not be compromised by the application of

conversion factors. Several tests were performed on traditional problem gases. Results

presented include C12, BC13, HBr, and WF6.

7
The impact of various gas properties on the operation of an MFC

Dan Mudd

Mass Flow Associates of Texas

Gas properties directly influence the operation of an MFC. Specific MFC components are influenced by specific gas properties and determine if the component is operating within

its linear region. Problems can arise with the use of surrogate gases as substitutes for

"nasty" nameplate gases if any MFC component is operated outside its linear region

when flowing either a surrogate calibration gas, the nameplate gas or a surrogate

transient-response gas. An evaluation of the gas properties and foot printing of the

individual components can suggest surrogate calibration practices and procedures to avoid miscalibrations seen in the industry associated with the use of surrogate gases by

MFC manufacturers. A review of the key gas properties affecting an MFC and their

effect on the individual MFC components is made.

NIST's program to measure the thermophysical properties of

semiconductor process gases

John J. Hurly and Michael R. Moldover

Process Measurements Division, National Institute of Standards and Technology

NIST has developed a facility to safely study the toxic, corrosive, and hazardous gases

that are used in the processing of semiconductors. We have completed measurements of

the speed of sound in the process gases CI2, HBr, BCI3, WF6, and (CF^O, and in the

surrogate gases SF6, CF4, and C2F6. The data span the temperature range from 200 K to 475 K and the pressure range from 25 kPa to the lesser of 1 500 kPa or 80% of the

sample's vapor pressure. The measurements are made along isotherms. Each isotherm is individually analyzed, and from the zero-pressure intercept the ideal-gas heat capacities

Cp{T) are obtained with uncertainties of 0.001 xCp(T). The slope and curvature of each

isotherm provides information about the gas's virial equation of state. The density virial coefficients are obtained by simultaneously fitting all the sound speed measurements to model pair and three-body intermolecular potentials. From the potentials, we can estimate

the viscosity 77(7) and the thermal conductivity A(7). The calculations extrapolate well

and extend to temperatures in excess of 800 K, well above the range of the

measurements. For gases where other data exist, we find the uncertainties in the

calculated properties are less than O.OOlxp, O.lxr], and O.lxA. We plan to measure 77(7)

and A(7), thereby reducing their uncertainties under 1 %. We plan to measure the

properties of the other gases that the semiconductor processing community identifies as having the highest priority. We have posted a trial version of a user-friendly database to disseminate the properties of process gases and carrier gases. This database can be found

at http://properties.nist.gov/SemiProp/. Please send comments concerning this database

to john.hurly@nist.gov.

S
Requirements for the next generation gas mass flow controllers

Kaveh Zarkar

Millipore Corporation

Continued advancement and improvements in the era of 0.25 |im and finer feature sizes

in semiconductor chip manufacturing have seen the advent of newer, faster and smaller

fluid handling components. Also, shifts in the industry trend from batch process to single

wafers has impacted the traditional gas system components. Future semiconductor

process capabilities, particularly the emerging demand for CVD and plasma etch,

eventually will affect the gas delivery systems and components, specifically the mass

flow controllers, which are important gas delivery components directly affecting the film

integrity and quality. Industry will require new and continuously improving generations

of MFCs that are superior in performance, more versatile in handling multiple gases, as well more reliable with reduced cost of ownership. To achieve the best results, gas

delivery component selection is going to play a vital role in achieving the tighter and

more demanding process requirements. This paper examines the specifics of each critical process as it relates to the MFC selection and functionality.

9
Participants in breakout sessions

Performance of flow meters

Gary Allen (leader) Applied Materials

Jeff Anastas MKS Instruments Robert Berg NIST

Daniel Coffman Applied Materials

Joel Derk Lucent

France D'Spain SW Research Institute Ed Francis XT i. ' 1 O " J < „ „ National Semiconductor

Tim Kipley Aera Corporation

Thomas Maginnis University of Massachusetts at Lowell

George Mattingly JNIS 1 Mike Munson Dominion Semiconductor

Thomas Naughton Dresser Equipment Group

Jeff Rose (assistant) Motorola

Greg Secord DH Instruments William White W3

Standards and calibration

Michael Bair Trace Beck

Brian Dickson

Gary Frank

Bill Johnson

William Kosh

James Long

Balarabe Mohammed

Daniel Mudd

George Porter William Valentine (leader)

Bob Williams

John Wright (assistant)

DH Instruments

International SEMATECH

Lucas Labs

Unit Instruments Eastman Kodak

Dresser Equipment Group

Aera Corporation

Applied Materials

Mass Flow Associates of Texas

Porter Instrument Co.

Unit Instruments

Coastal Instruments NIST

Gas properties

William Alvesteffer Wang Chiun

James Hardy (assistant)

John Hurly (leader)

Jim Hylton

Max Klein

Jack Martinez

Gil Yetter

Teledyne Hastings

Unit Instruments Oak Ridge National Laboratory

NIST

Bechtel Jacobs Company LLC

Scitefair International, Inc. NIST

International SEMATECH

Alternatives to

Chris Davis

Joe Dille David Green

Bin Han

Albert Henning

Michael Moldover (assistant)

Maceo Ward

Kaveh Zarkar (leader)

Jay Zemel

thermal mass flow controllers

FuGasity

Brooks Instrument NIST

MKS Instruments Redwood Microsystems

NIST

Millipore Corporation

Millipore Corporation

Scitefair International, Inc.
Discussions in the full workshop

The next four subsections summarize the discussions held in the full workshop. The

context for these discussions consisted of six presentations, whose slides are reproduced

in Appendix F, and the discussions in the breakout groups. Many discussions led to the

proposal of a specific task. The list of tasks in Appendix A gives a summary of these

topics. This section explains why some of the tasks were proposed, and it provides brief

accounts of discussions that did not lead to proposed tasks.

Performance of flow meters

The breakout group used a recent article to estimate future MFC requirements (Kaveh

Zarkar, "Requirements for next-generation gas-flow components", Solid State

Technology, March 2000, pp. 27-32). Table 1 of this article listed improvement factors

expected for MFC requirements by 2004. The table below applies Zarkar' s improvement

factors to Applied Materials' present MFC requirements. Four of the requirements in 2000 are listed on slide 10 of Gary Allen's presentation (Appendix F). The other rows

(turndown ratio, overshoot, and settling time) were written down after discussions in the

breakout group.

Characteristic Requirement in 2000 Requirement in 2004

accuracy 1% of full scale 0.5% of full scale

repeatability 0.25% of full scale 0.13% of full scale

valve leak 1% of full scale 0.3% of full scale

turndown ratio 20 80

overshoot 10% of set point 2% of set point

step response 1.5 s 0.3 s settling time 2 s 1 s

The attendees generally agreed with this table. However, one representative of an MFC

manufacturer asked if the desired requirements were driven more by measurement

feasibility than by the needs of the manufacturing processes. Several examples of process

needs were given in response, one of which was tungsten deposition requiring a 1-second

step response with no overshoot. One participant made the general point that improved

MFCs will enable new processes.

The attendees characterized the most important MFC requirement as interchangeability,

which means that replacing one MFC with another MFC designed for the same flow rate has negligible effect on the manufactured product. Interchangeability comprises the

requirements of accuracy, linearity, and reproducibility. Several participants emphasized

that the MFCs must be interchangeable for transient as well as for steady flows. One

participant pointed out that the interchangeability of MFCs from the same manufacturer

is easier to achieve than interchangeability of MFCs from different manufacturers. Due to differences in design and calibration, the interchangeability of two MFCs from different

manufacturers seems unlikely unless both MFCs have accuracies better than the required

interchangeability.

1 1
One representative of an MFC manufacturer stated that there is little demand for MFCs

that operate at low flow rates. Others disagreed, saying that demand is increasing, or saying that demand would be greater if the MFCs were more reliable at low flow rates. Problems common at low flow rates, such as long gas delivery lines and poorly

controlled valve sequencing, make it difficult to verify such reliability. Severalparticipants stated that standards at low flow rates would be helpful here. Another

comment was that accurate flow control is needed for recipes requiring stochiometry

ratios exceeding 100:1.

A benign surrogate gas, such as SF6, is frequently used to calibrate an MFC intended for

a difficult process gas, such as WF6. Different MFC manufacturers use different sets of

surrogate gases, which can complicate the comparison of MFCs from different

manufacturers. Many participants advocated that every MFC manufacturer characterize

each MFC's performance with nitrogen, even if nitrogen was not the calibration gas. This

would allow a simple verification that the MFC was working properly, both at the tool

manufacturer as well as at the semiconductor fabrication plant, even if the MFC was not

intended for use with nitrogen. The cost of such characterization was not clear.

Other issues considered included the following.

• Better techniques to measure gas flows at subatmospheric pressures are needed.

• Characterization of an MFC for the process gas is best done by a function of flow

rate instead of by a flow-independent "gas correction factor".

• Frustration exists with MFC zeros that are set either incorrectly or inconsistently.

Standards and calibration

The breakout group called for the following new or improved tests and standards.

• Transient flows and crosstalk due to pressure variations.

• An "in situ" standard for process gases accurate to 1 % between 0.01 seem and

1000 seem.

• Liquid flows below 15 ml/minute.

• Transfer standards between 0.01 seem and 1000 slm for "round robin"

(inteiiaboratory) tests.

The group also called for clarification in two areas.

• The phrase "NIST traceable" needs to be made more meaningful. This was

motivated by John Wright's distinction between direct and indirect traceability

.

Several participants pointed out that "NIST traceable" is widely abused.

• Documents are needed on the "best practice" for various primary standards,

similar to those produced by the National Conference of Standards Laboratories.

The existence of SEMI standards for MFC testing needs to be publicized better.

Many participants emphasized the desirability of calibrating an MFC with the intended

process gas instead of a benign surrogate gas. While more expensive, such "live gas"

calibration improves the MFC's accuracy, thereby reducing the cost of "tweaking in" a new process on the semiconductor manufacturing tool. The participants identified only

12
four facilities for live gas testing. The first, at a government laboratory (Oak Ridge

National Laboratory), has been little used in recent years. The others are at a commercial

testing laboratory (W3 Corporation) and at two MFC manufacturers (Kinetics and

Millipore). One process engineer suggested approaching end users such as himself for

help. A widely accepted cost-benefit analysis of live gas calibration does not exist.

Gas properties

The thermophysical properties of process gases have a direct effect on the design,

calibration, and operation of MFCs. The large uncertainties associated with the gas

properties of many process gases make the improvement of MFC models more difficult. The accuracy required of a property depends on how the MFC's performance is affected

by that property. For example, for a thermal MFC the most important property is the heat

capacity at constant pressure, but for a sonic nozzle MFC it is the speed of sound. Three

improvements were discussed.

• Direct experimental measurements of properties. The Fluid Science Group at NIST is characterizing four to ten semiconductor process gases per year with

accuracies sufficient for thermal MFCs (for example, 0.1% in heat capacity and

0.5% in viscosity).

• Development and application of techniques to estimate properties. This will

provide property values much faster than the measurements at the cost of worse

accuracy. The associated uncertainties are expected to be approximately 20 times

larger than for direct measurements, and the techniques require at least a few

measurements for their validation and improvement.

• Compilation of existing property values, both measured and estimated, in an

easily accessible database.

The importance of mixture properties was unclear. MFCs that prepare a mixture by

controlling the flow of pure gases do not require the properties of the mixture created

downstream. MFCs that control the flow of a dilute mixture (for example, a small amount

of O2 in He) may require the mixture's properties, but they are easily estimated from the

properties of the pure components because the mixture is dilute. NIST is not aware of any

process that requires the flow control of a concentrated mixture. The identification of

such processes would be extremely valuable.

The breakout group recommended development of a generic MFC model, starting with

components such as the flow divider. This recommendation, which was discussed twice

earlier in the contexts of gas correction factors and of surrogate gases, was controversial.

Attendees representing MFC manufacturers noted that MFC designs are proprietary.

Alternatives to thermal mass flow controllers

The breakout group used a matrix approach to think about competing flow measurement

techniques. One side of the matrix listed measurement techniques, including thermal

MFCs. The other side listed manufacturing processes, examples of which can be found in Kaveh Zarkar's presentation (Appendix F). In principle, each cell of the matrix could be

filled with an assessment of the suitability of a particular technique for a particular

process. In practice, this could not be done during the workshop because it would have

13
required detailed knowledge of the processes and their fluids as well as the techniques.

Examples of such details include the following.

• process

operating pressure

flow requirements

flow dynamics

step time requirement

• fluid

precursor phase (solid, liquid, gas, vapor)

chemical compatibility

density

specific heat

vapor pressure

Predicting the future suitability of the techniques was even more difficult. Alternatives to thermal MFCs have capabilities that are still being developed, and new manufacturing

processes continue to immerge. The panel recommended that SEMI, NIST, and the

semiconductor industry work together to characterize the new processes and fluids.

The breakout group concluded that NIST can help the development of new flow

measurement techniques in the following ways.

• Provide flow standards suitable for new techniques.

• Provide property data for new process gases.

• Use scientific understanding to improve existing techniques. A recent example is the identification of molecular relaxation effects in sonic nozzles.

• Develop new techniques.

14
Final recommendations

Of the 21 proposed tasks listed in the Appendix A, seven received a vote from at least 40 % of the non-NIST attendees. These strongly recommended tasks are listed in the

table on the next page. Each of the other 14 tasks received a vote from less than 25% of

the attendees.

Five of the seven strongly recommended tasks require action by NIST. As part of NIST's

Chemical Science and Technology Laboratory (CSTL), the Process Measurements

Division uses six guiding criteria to set program priorities. The workshop's

recommendations are discussed below in relation to these criteria.

1. The magnitude and immediacy of the industrial need.

The industrial interest in this workshop showed that the industrial need for gas property

values and flow standards is immediate and at least moderate. The rapid introduction of

new processes by the semiconductor industry may make the need more urgent.

2. The degree of correspondence between a particular industrial need and CSTL's

mission.

The degree of correspondence is high. Providing reference standards for flow and

property values for pure, industrially important fluids will fulfill CSTL's mission by

enhancing the productivity of U.S. industry.

3. The opportunity for CSTL participation to make a major difference.

CSTL's participation will make a major difference for two reasons. First, CSTL is the

premier source for the thermophysical properties of gases. Second, NIST's reputation as an unbiased, reliable provider of reference standards for flow and other quantities makes

it likely that the proposed flow standards will be used by industry.

4. The nature and size of the anticipated impact resulting from CSTL's

participation.

CSTL has the capability to match most of the industrial needs. See criteria 1 and 2.

5. CSTL's capability to respond in a timely fashion with a high-quality solution.

CSTL's capability to respond is large because many of the needs match existing

programs or expertise in CSTL. Tasks 4, 5, and 6 correspond to programs in the Process

Measurements Division. Tasks 1 and 3 correspond to recent work done in the Division.

6. The nature of opportunities afforded by recent advances in science and

technology.

The opportunities are significant and numerous. The gas property measurements rely on

acoustic techniques recently developed and under constant improvement at NIST. The

existing transfer standard for low flow rates of gases relies on recent advances at NIST in modeling laminar flow elements.

15
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Appendices

A. Prioritization of the proposed tasks

The following tables show the tasks proposed by the breakout groups and their

prioritization by the attendees. Most proposals also specify the institution that would

accomplish the task. The tasks are reworded here to improve the descriptions written on

flipcharts during the workshop.

Each attendee was allowed to vote for six tasks without voting more than once per task. The votes ofNIST attendees are excludedfrom the tables.

We emphasize that all of the tasks were proposed only after discussion in the full workshop as well as in the breakout groups. Thus, even those tasks with few votes

deserve serious consideration.

Performance of flow meters

Task Institution Votes

Write standard on procedure for adjusting MFC zero. SEMI 6

Devise a technique to verify MFC performance that is independent of the process chamber. none specified 14

Characterize the performance of each new MFC with

nitrogen as well as with its nameplate gas. MFC manufacturers 23

Develop techniques to characterize delivery of gas

below atmospheric pressure.

NIST 4

Standards and calibration

Write document on best practices for primary standards. NIST 6

Develop a facility and methods for testing transient

performance.

NIST 3

Increase the range of transfer standards for conducting

round-robin tests (0.01 seem to 1000 slm).

NIST 24

Improve the primary (0.025%) and transfer (0.1%)

standards for gas flow.

NIST 27

Develop a test facility for corrosive and toxic gases. none specified 4

Develop primary standards for liquid flows below 15

ml/min. (TEOS, TMB, etc.)

NIST 8

17
Gas properties

Task Institution Votes

i—i i i

• , • , i i• , e* i 1*1 Expand and repriontize the list of gases to be studied.

Schedule and conduct property measurements.

NIST 20

f*l 1 * j 1 1 . . • Supplement experimental measurements by estimating,

with uncertainties, the properties of pure gases.

NIST 6

Establish and maintain a public, Web-based database of

gas properties.

NIST 20

Create an industry advisory board to guide NIST. MFC manufacturers,

tool manufacturers,

MFC users

5

Develop a generic MFC model. Suggested first submodels: sensor, flow restrictor, transient response.MFC manufacturers,

NIST

6

Identify important gas mixtures. Estimate, with

uncertainties, their properties. (Industry survey,

literature search, measurements.)

NIST 5

Alternatives to thermal mass flow controllers

Identify processes likely to be important. SEMI 2

Identify chemical precursors likely to be important. SEMI 1

Create a database of precursor properties. NIST 1

Identify the flow ranges likely to be important. SEMI 0

Develop metrology to characterize liquid flow

controllers

NIST 19

18
B. Suggested topics for breakout sessions

1 . Flow meter performance

1.1. Industries

1.1.1. semiconductor device manufacturing

1.1.2. others: air pollution, pharmaceuticals, leak testing, . .

.

1.2. Process conditions

1.2.1. flow rate

1.2.2. fluid composition

1.2.3. pressure (including transients)

1.2.4. temperature

1.2.5. corrosion

1.3. Requirements

1.3.1. accuracy

1.3.2. stability (repeatability)

1 .3.3. dynamic range

1.3.4. interchangeability

1.4. Challenges from new processes

1 .4. 1 . lower flow rates

1 .4.2. pressures below one atmosphere

1.4.3. new fluids (gas mixtures, high temperature vapors, liquids)

2. Standards and calibration

2.1. Requirements

2.1.1. flow rate

2.1.2. uncertainty

2.1.3. traceability

2. 1 .4. relation of surrogate gas to process gas

2. 1 .5. location (standards lab, MFC manufacturer, process tool)

2.2. Primary flow standards

2.2.1. gravimetric (weighing)

2.2.2. constant volume (pressure rate-of-rise)

2.2.3. constant pressure (piston prover)

2.3. Transfer flow standards

2.3. 1 . pressure drop across a laminar flow impedance

2.3.2. thermal MFC

2.4. Research at national laboratories

2.4. 1 . improved flow standards

2.4.2. new standards (transient flow, mixtures)

2.4.3. validation of MFC models by comparison of process and surrogate gases

2.4.4. MFC corrosion and reliability testing

2.5. SEMI guidelines and test methods

2.5.1. practical implementation

2.5.2. validation

19
Gas properties

3.1. Influence of properties on MFC models

3.2. Property measurements

3.2.1. thermodynamic (heat capacity, compressibility, virial coefficients)

3.2.2. transport (viscosity, thermal conductivity)

3.2.3. other (speed of sound, Prandtl number)

3.3. Property models

3.3.1. prediction from molecular structure

3.3.2. mixture properties

3.3.3. sources of reliable data and correlations

3.4. Generic modeling of dynamics

3.4.1. hydrodynamics

3.4.2. slip

3.4.3. thermal diffusion

3.4.4. molecular relaxation rates

Alternatives to thermal mass flow controllers

4.1. Micro-electrical-mechanical systems (MEMS)

4.2. Pressure drop across a laminar flow impedance

4.3. Sonic nozzle

4.4. Conolis effect

4.5. Acoustic

C. Abbreviations and jargon

CD

CSTL

MFC

nameplate gas

NIST

round robin

seem

SEMI

critical dimension

Chemical Science and Technology Laboratory

mass flow controller

The process gas named on the body of the MFC.

National Institute of Standards and Technology

A scheme to compare laboratory measurement capabilities in

which a test artifact is circulated among the laboratories.

standard cubic centimeter per minute (= 1 .34 |imol/s)

Semiconductor Equipment and Materials International

semiconductor tool Work station for deposition on and etching of semiconductor

wafers, including a process chamber and a gas handling system

slm

20

standard cubic liter per minute (1000 seem)
D. Workshop schedule

Monday, May 15

8:30 Introductions

9:00 Talks to outline the issues

• Performance offlow meters

Gary Allen, Applied Materials

• Standards and calibration

John Wright, NIST

Bill Valentine, Kinetics

10:15 Coffee

• Gas properties

Dan Mudd, Mass Flow Associates of Texas

John Hurly, NIST

• Alternatives to thermal massflow controllers

Kaveh Zarkar, Millipore

12:00 Guidelines for breakout sessions

12:15 Lunch

1:15 Breakout sessions

3:00 Coffee

5:00 Adjournment

6:00 Social hour

7:00 Dinner

Tuesday, May 16

8:30 Reports from breakout sessions

10:15 Coffee

1 1 00 Final breakout sessions

12:15 Lunch

1:15 Prioritization of recommendations

3:00 Adjournment

3:30 Tours of NIST flow facilities
E. Participant addresses

Gary Allen Applied Materials 2901 Patrick Henry Dr. MS 5509

Santa Clara, CA 95054 USA

Telephone: 408/986-3436

Fax: 408/563-6114

gary_allen@amat.com

William Alvesteffer TET Hastings Instruments

P.O. Box 1436

Hampton, VA 23661 USA

Telephone: 757/723-6531

Fax: 757/723-3925

walveste@teledyne.com

Jeffrey Anastas MKS Instruments 651 Lowell St. Methuen, MA 01844 USA

Telephone: 978/682-4567

Fax: 978/682-4956

jvanastas@yahoo.com

Mike Bair DH Instruments, Inc. 1905 West 3rd St. Tempe, AZ 85281 USA

Telephone: 480/967-1555

Fax: 480/968-3574

dhi@dhinstruments.com

Trace Beck

Int l. SEMATECH

2706 Montopolis Dr. Austin, TX 78741 USA

Telephone: 512/356-7609

Fax: 512/356-7008

trace.beck@sematech.org

Bobby Berg

NIST

100 Bureau Drive

Mail Stop 8364

Gaithersburg, MD

20899-8364 USA

Telephone: 301/975-2466

robert.berg@nist.gov

Daniel Coffman

Applied Materials 9700 U.S. Hwy.

2900 East MS/3100-183

Austin, TX 78724 USA

Telephone: 512/272-2979

Fax: 512/272-3060

danJ_coffman @ amat.com

France D'Spain

SW Research Institute 6220 Culebra Rd. San Antonio, TX 78238 USA

Telephone: 210/522-2979

Fax: 210/522-3658

fdspain@swri.org

Christopher Davis

FuGasity

616 Huntington Lane

Allen, TX 75002 USA

Telephone: 214/679-5380

Fax: 775/358-0434

fugasity@aol.com

Joel Derk

Lucent Technologies

555 Union Blvd. Allentown, PA 181 03 USA

Telephone: 610/712-7550

Fax: 610/712-7513

jlderk@lucent.com

Brian Dickson Lucas Labs

393-J Tomkins Court

Gilroy, CA 95020 USA

Telephone: 408/846-1402

Fax: 408/848-3352

lucaslabsl@aol.com

Joe Dille Brooks Instrument 407 W. Vine St. Hatfield, PA 19440 USA

Telephone: 215/362-3523

Fax: 215/362-3745

joe.dille@frco.com

Ed Francis

Natl. Semiconductor Corp. 1111 West Bardin Rd.

Arlington, TX 76017 USA

Telephone: 817/468-6522

Fax: 817/557-7644

ed.francis@nsc.com

Gary Frank

Unit Instruments/Kinetics

Fluid Sys.

22600 Savi Ranch Pkwy.

Yorba Linda, CA 92887 USA

Telephone: 714/921-2640

Fax: 714/921-0985

gfrank@kineticsgroup.com

David Green

NIST

100 Bureau Drive Gaithersburg, MD 20899-

8364 USA

'

Telephone: 301/975-4869

david.green @ nist.gov

22
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Mill Ctnn QQCfl Mail otop oobU James Long Mass Flow Associates of GaithGrsburg, MD Acra Corporation Texas

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George Porter William White

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Fax: 215/723-2199 Telephone: 775/358-2332

georgeporter® Fax: 775/358-0434

porterinstrument.com bill@w3corp.sparks.nv.us

Jeff Rose Bob Williams

Motorola Coastal Instruments, Inc. 3501 Ed Bluestein Blvd. P.O. Box 577

MD-K10 Burgaw, NC 28425 USA

Austin, TX 78741 USA Telephone: 910/259-4485

Telephone: 512/933-5599 Fax: 910/259-3375

Fax: 512/933-5262 bobw@mfchelp.com

rtla30@email.sps.mot.com

John Wright

Greg Secord NIST

DH Instruments, Inc. 100 Bureau Drive 1905 West 3rd St. Gaithersburg, MD 20899 USA

Tempe, AZ 85281 USA Telephone: 301/975-5937

Telephone: 480/967-1555 john.wright@nist.gov

Fax: 480/968-3574

dhi@dhinstruments.com Gil Yetter

Intl. SEMATECH

Bill Valentine 2706 Montopolis Dr. Kinetics Fluid Systems Austin, TX 78741 USA

22600 Savi Ranch Pkwy. Telephone: 512/356-3227

Yorba Linda, CA 92887 USA Fax: 512/356-7008

Telephone: 714/921-2640 gil.yetter@sematech.org

Fax: 714/921-1749

bvalentine© Kaveh Zarkar

kineticsgroup.com Millipore Corp.

915 Enterprise Blvd. Chiun Wang Allen, TX 7501 3 USA

Unit Instruments/Kinetics Telephone: 972/359-4000

Fluid Sys. Fax: 972/359-4107

22600 Savi Ranch Pkwy. kaveh_zarkar@ millipore.com

Yorba Linda, CA 92887 USA

Telephone: 714/921-2640 Jay Zemel

Fax: 714/921-0985 Scitefair International, Inc. cwang@kineticsgroup.com 3508 Market St. Ste. 35

Maceo Ward Philadelphia, PA 19104 USA

Millipore Telephone: 215/382-5690

915 Enterprise Blvd. Fax: 215/382-5691

Allen, TX 75013 USA zemel@ee.upenn.edu

Telephone: 972/359-4502

Fax: 972/359-4106

maceo_ward@millipore.com

24
F. Presentation viewgraphs

Mass flow controller performance and characterization

Gary Allen, Applied Materials

Gas flow standards and calibration

John Wright, NIST

Consistent ±3 sigma calibration

Bill Valentine, Kinetics Fluid Systems

The impact of various gas properties on the operation of an MFC

Dan Mudd, Mass Flow Associates of Texas

NIST's program to measure the thermophysical properties of

semiconductor process gases

John Hurly, NIST

Flow controllerfor semiconductor industry

Kaveh Zarkar, Millipore

25
NIST Workshop - Mass flow measurement &

control for the semiconductor industry

MFC Characteristics and Behavior

May 15th, 2000

Gary Allen

Applied Materials

Technology Engineer

Fluid Systems Development

Topics

1) Definitions & Flow Terminology

2) MFC Types & Internal Components

3) AMAT Testing & Requirements

4) Gases and Surrogate gases

5) Comparative Performance Data

• Analog MFC vs D/A MFC vs DeviceNet MFC

6) Issues and Concerns

7) New MFC Capabilities

8) Conclusions

9) Discussion / Questions
MFC Definitions & Terminology

Analoa MFC Sensor offset

Diaital / Analoa MFC Sensor drift DeviceNet diaital MFC Repeatability

Transient characteristics Reproducibility

Dead time Cross talk

Step response time Thermal Based

Control (settling} time Pressure Based

Overshoot Coriolis Based

Accuracy (% FS)

Linearitv

Valve leak by

MFC Types and Internal Components

• MFC types - Thermal based - Pressure based - Coriolis - MEMS

• Internal Components

- sensor - valves - bypass - control logic
Testing Requirements

AMAT MFC Commodity Specification - P/N 0251 -00345 ; defines the minimum set of

requirements for MFC configuration, performance and

reliability.

Applied Materials tests performance of MFC types

and models via RoR system. - creates a common test method for comparative analysis - measures transient flow characteristics of MFCs

- limited to 3 SLM

AMAT Performance Characterization

• Tests specific performance characteristics for compliance to AMAT MFC Commodity Specification (p/n 0251-00345)

• Test for nine different characteristics - dead time, step response time, control time, overshoot, accuracy,

valve leak-by - calculate - linearity, repeatability, reproducibility

• Nine different set points (2% to 100%) repeated three times

• Four different test gases are utilized (N2, He, CF4, SF6)

- Typical inlet pressure 30 psia - Initial chamber pressure 35 mTorr

• Tests each MFC independently.

• Sample rate 25 mSec.
Gases & Surrogate Gases

• The Semiconductor industry utilizes approximately

170 different gases, in which the list grows every

year.

• SEMI published list E52-95 "Practice for

Referencing Gases used in Digital Mass Flow

Controllers.

• Gases run the gamut of inert, toxic, corrosive,

flammable, vapor from liquids, liquids, and solids

• MFCs are not calibrated with the the name plate gas.

• Typically a GCF gas correction factor is applied

linearly for the surrogate to name plate gas.

APPLIED MATERIALS'1

Gases & Surrogate Gases

Issues with surrogate gases

• Correlations between name pate gases and

surrogate gases are not linear, therefore GCFs can

cause inaccuracies.

• Applied has found multiple cases of GCFs being

inaccurate. In some cases these have been as high

as 8%FS.

• Different manufacturers utilize different surrogate

gas for calibration.
Gases & Surrogate Gases

Digital MFCs are utilizing gas correction functions to

eliminate linearity issues of gas correction factors.

Some gas correction functions are theoretical, while

others are derived from empirical testing.

Live gas testing allows for these gas correction

functions to be developed, and appear to generate

the best correlations.

We recommend that MFC manufacturers develop

these non-linear relationships to only one surrogate

gas - Nitrogen.

APPLIED MATERIALS*

Performance Comparison

Analog MFC* L>AMFC# De\riceNetMFC# 1.13 DNet MFC*l Characteristic Spec Requ'rerrat i

CeedTime NfTlsec 0.35 sec Q31 sec Q18sec Q2sec

Step Ftesp Time 1.5 Sec Q72sec Q91sec 1.01 sec Q71 sec

Setting Time 20 Sec 1.30 sec 1.18 sec 1.92 sec 1.551 sec Oersted 10%SetFtirt 7.95% 508% 460% 343%

Vai\e Leak-by 1%FS 0.03% Q32% Q18% 011%

tocuacy 1%PS Q38% 075% Q78% 045%

Linearity 1%FS Q39% 081% 052% 049%

F^peatablity .25% PS rocfetaaailarJe 022% 009% 005%

F^prcdxiblity MR 1%FS 1.74% 1.40% Q70% Q62%

j _
New MFC capabilities

• Improved calibrations - through the use of gas correction functions derived

through live gas empirical data, Polynomial equations

determine calibration curves rather than a single point

linear relation between surrogate gas and name plate gas.

• Multiple gas calibrations - can be stored in a single MFC, which allows for capability

of reduced inventories.

• Common communication protocols - allow for enhanced diagnostics - easier integration

Issues and Concerns

Cross-talk - a pressure fluctuation in a SLD manifold

which causes MFC flow output to vary.

Regulator interaction - improperly functioning

mechanical pressure regulators can affect transient

behavior of MFC.

Gas Bursting - uncontrolled amounts of gas, caused

by various MFC interaction with semiconductor tools.

In situ flow verification - a means to verify gas flow on

the semiconductor tools, independent to the process

chamber.
Issues and Concerns

Pressure based MFC

- potential" down stream" Crosstalk? - continuous sonic velocity concern? - inlet pressure concern?

Liquid Delivery Measurement

- measure in liquid or vapor phase? - transient characteristics?

SDS Delivery Systems

- experimental methods limited - dealing with low differential pressures

Conclusions

• Digital MFCs have improved performance and capability over

existing analog MFCs.

• Comparative performance evaluations and interactive

feedback have improved the capabilities of MFCs in the past

three years.

• Gas correction functions should be verified by some level of

live gas testing.

• More work has to be completed to understand the interaction

of inlet & outlet pressure, relative to transient characteristics &

accuracy.

• Transient measurement techniques must be developed for

liquid and SDS MFCs.
Gas Flow Standards

and Calibration

John D. Wright

Project Leader

Fluid Flow Group

N^tinnpl i 'Ja uui 'til In^titnto ii lolilL'lc nfUl O^tanHarrtc Idl lUdl Uo and dl lU Tor^hnnlnm/ 1 til II IVJ 1 UU y Gaithersburg, MO, USA

www. nist.go v/fluid_ flo w outline

Outline

• Mission

• Flow standards

• Traceability and Proficiency

• Inter-lab comparisons

www,nist. gov/fluid_ flo w gas standards |

33
Mission

• Support industry by maintaining and

disseminating measurement standards

• Improve uncertainty of primary flow

standards as needed by industry

• Conduct calibrations, inter-lab

comparisons (international and domestic)

• Flowmeter research for transfer standards

www.nis t.go v/fluid_ flo w

NIST Pressure and Vacuum Group

Improved gas flow calibrations from 0.01 to 1000 seem

• Primary standards

- first-generation

• constant volume; pressure rate-of-nse

• 0. 1 % in practice - second-generation

• constant pressure; volume displacement measured by laser interferometer

• approximately 0.05% expected

• Transfer standards based on a laminar flow impedance

- first-generation (rectangular cross-section)

• good reproducibility (short-term is 0.005%, long-term is at least 0. 1 %)

• new model has minimal empiricism (only free parameter is duct diameter) - second-generation (circular cross-section) completed

• New directions - Workshop on mass flow control - Investigation of acoustic flow meter as a measurement standard

34
35
LFE model: R.F. Berg and S.A. Tison (2000)

1.00

•c

0.99

I - I I.. I J.I III I 1

' * I 1 1 1

1 |

i I I I i 1 1

1 | |

i i i i i il | |i 1111 0.01 0.1 1 10 100 1000

Reynolds number

NIST Fluid Flow Group

Gas Flow Standards

Facility Min. Flow

[slm]

Max. Flow

[slm]

U (k=2)

[%]

Fluid

Small Piston 3.72e-2 5.22e-1 0.19 Non-Corrosive Medium Piston 2.03e-1 2.84e+0 0.16 Non-Toxic Large Piston 2.12e+0 2.97e+1 0.18 Gases

Non-Corrosive GVC 1.00e+0 1.00e+3 0.05 Non-Toxic Gases Small Bell 1.61e+1 2.26e+2 Non-Corrosive Medium Bell 3.05e+1 4.55e+2 0.17 Non-Toxic Large Bell 1 .03e+2 1 .44e+3 Gases

PVTt 8.62e+2 7.76e+4 0.20 Dry-Air

www,nist. gov/fluid_ flo w
Piston Provers

Min. Flow Max. Flow U (k=2) Fluid

[slm] [slm] [%]

www, n is t. go v/fl uid_flow

3.72e-2

2.03e-1 2.12e+0

5.22e-1 2.84e+0

2.97e+1

0.19

0.16

0.18

Non-Corrosive Non-Toxic Gases

Gravimetric-Volumetric Calibrator (GVC)

II

9 9

O

O ©

9 9

9 9

Min. Flow Max. Flow U (k=2) Fluid [slm] [slm] [%]

1.00e+0 1.60e+3 0.050 Non-Toxic cases www.nist. gov/fluid_ flow
Min. Flow Max. Flow U (k=2) Fluid

[slm] [slm] [%]

8.62e+2 7.76e+4 0.20 Dry-Air www.nist.gov/fluid_flow
Traceability

• A measurement or sensor is said to be

traceable if it can be connected to a

stated reference, usually a national

standard, through an unbroken chain of

documented calibrations with stated

uncertainties.

• May be indirect or direct.

International Vocabulary of Basic and General Terms in Metrology, 2nd edition, International Organization for

Standardization, 1993. www.nis t.go v/fluid_ flow

Proficiency

• A laboratory proves proficiency by

having well founded and performed

calibration procedures and by

demonstrating agreement with other

laboratories via comparisons.

Calibration Laboratories Technical Guide,

C. D. Faison, editor, NIST Handbook 150-2, 1997.

www.nist.gov/fluid_flow
Fluid Flow Group Inter-lab

Comparisons

X

X

PVG 3/V6 NRLM 4/% A PVG 3/97 A NPSL l»X CEESI >OTX X CENAM 1 1/98 •CEESI IW

-NEL IW

O KRISS i/W CMS 1AW 0 NRLM

I (XXX) 1 00000 Flow (L/min)

Sematech Round Robin, 1993

1.1

1.08

cvf ~ 1.06

ti> |l.04h

2

a

CLJ 0.98

El^0.96

"5io.94 o2

0.92

0.9

1 1 1 r

] rp

[l' 'J

, i 1 i i i i 0.92 0.94 0.96 0.98 1 1.02 1.04 1.06 1.08 Nonral'eed Flow Rate Ratio (Config. 1-3)

www.nist.gov/fluid_flow

40
Sematech Round Robin, 1993

1.01

1.008

1.006

at ^1.004 = 1.002-

<r

DC10.996 J

0596

"5§ 0.994- o

0.992

0.99

0.99

www.nis t.go v/fluid_ flo w

C

|:

4*-

r R

8

• u-q0595 1 1.005 Normalized Row Rate Ratio (Config. 1-3) 1.01

Summary

• primary gas flow standards are

being improved

• both traceability and

proficiency are important

• comparisons ensure quality,

check entire calibration

process

www,nis t. qov/fluid_ flow end
Kinetics Fluid Systems

Consistent +/- 3 Sigma Calibration

Bill Valentine, Director of Engineering

^KINETICS

1% FS Accuracy?

• Claimed since the beginning of the MFC

• Past: 70% of product met an accuracy of

1 % FS on surrogate gas. (1 sigma process)

• Goal: 99.7% of product would meet an

accuracy of 1% FS on surrogate gas AND

process gas

• Now shipping product with % SP accuracy

^KINETICS
Do you understand your

capabilities and limitations,

or do you just feel lucky?

^KINETICS

3 Tier Attack

Metrology

- Do we have a solid foundation?

Process Capability

- Are we under control?

On Tool Performance

- Can we translate solid metrology and process

capability into on tool performance?

^KINETICS

43
METROLOGY

He who has one flow standard always

knows the flow rate.

He who has two flow standards, never

knows the flow rate.

^KINETICS

Without cross-checking different primary calibrators which do not share the same error sources, high confidence in flow accuracy cannot be maintained

Using

Ail

the Tools
Gravimetric Primary Calibrator

V4 V2

disconnect to weigh accurately

V1 v

V3 m

Strengths: Simple in principle, few

variables, any gas

Difficulties: Large tare + low gas mass

long run times, batch device, not commercially available. m = (m2

- mi) / At (gm/min)

KINETICS

Volumetric Primary Calibrator

Strengths: Commonly available,

operates at atmospheric pressure.

Difficulties: Determining barometric pressure accurately, needs

maintenance, only non-reactive gas, sealing fluid issues, batch device.

i Op

m= M P AV / (82.056 Z T At) (gm/min)

^KINETICS
Bell Provers

^KINETICS

Rate-of-Rise Primary Calibrator

P T

Strengths: Rugged,

moveable, use with any

gas.

Difficulties: Determining

volume, pressure, gas

temperature, configuration

induced uncertainties, batch

device.

Hj M TTJ m= M V AP/ (82.056 ZT At) (gm/min)

€r: i KINETICS
Critical Flow Nozzles

Strengths: Very small, very

stable, robust, excellent at intermediate flows, continuous

reading.

Difficulties: Initial characterization, data reduction, limited-gases and

ranges, pressure drop.

T

m = Cd C* At P0

/ V(RT) (gm/min)

kinetics

Laminar Flow Elements

Strengths: Very stable if handled

well, continuous reading, linear, excellent at all semi industry flows.

T

Difficulties: Initial characterization,

temperature effects, pressure drop.

Qs = C P AP D

4

/ ((iLTZ) (seem)

^KINETICS
Calibration Chain of Traceability at Unit Instruments

NIST Fluid

Laboratory Flow H

Variable Pressure

Primary

Degrading Accuracy

Critical ^ Flow

Nozzles

Variable Volume

Primary

( Laminar

•j Flow

I Elements

Production MFCs;;, [j

Gravimetric

Calibrators

Uncertainties among primary calibrators at Unit Instruments are now known to 0. 1 %

^KINETICS

\ Capable Call brati on Process

(Equal Area Curves)

percent calibration error

^KINETICS
Determining Calibration Capability

1 .Set Calibration

Initial Calibrator A

3. Measure Calibration

Screening

Calibrator B 1

2. Move MFC to

[ another calibrator pfl

: . =

^_

4. Subtract initial calibration errors from screening

measurements to determine

repeatability of MFC plus

calibration system errors.

5. After hundreds of measurements on all gases

and ranges in normal

production runs, calculate standard deviation of errors.

^rJ KINETICS

Reproducibility of New Calibration System and Repeatability

of MFC in % Full Scale

Peya!i<?n ?l FiM C?l l? Serening —< 2 STD

20% 40% 60% 80% 100% 12 >%

^KINETICS
Actual Calibration Data vs. the

Normal Distribution

Average of all calibration

points, 1050 MFCs, a=0.203

€^ KINETICS

ON TOOL PERFORMANCE

• Process gas calibration is not feasible

• Conversion factors

- Must understand your device and it must be

linear

• Gravimetric

- Characterization, not to generate a function

• Proof

- BCI3, CI2, WF6, HBr

^KINETICS

50
"Ability to precisely change calibration and tuning for different gases and ranges without lab re-calibration." Multigas / Multirange

-3%

—

9

Setpoint, Percent of Full Scale

300 seem N2

• 420 seem He

-80 seem SF6 — 1 00 seem N2 — 1 40 seem He

-26.7 seem S F6

fei KINETICS

o

Ql

hLU05

o1 UJ

"Superior linearity and accuracy on 'difficult' gases: BCL3, CI2"

Difficult Gases: Chlorine

1 .00%

0.75%

0.50%

0.25%

0.00%

-0.25%

-0.50%

-0.75%

-1.00%

CI2 Flow Error

Set Point (% FS)

€d KINETICS
Difficult Gases: BCIo

a.hLU

CO

O1

lij

1.00%

0.75%

0.50%

0.25%

0.00%

0.25%

0.50%

0.75% \

1.00%

BCI3 Flow Error

"Superior linearity and accuracy on 'difficult' gases:

BCL3, CI2"

io„ -9g_

—=—961 0085400 9610085500

Set Point (% FS)

^KINETICS

Multi-Gas MFCs: a Reality

Metrology Report, UFC-1661, 200 seem WF6

Primary

Calibrator:

Bell Prover

#109

Bell Prover

#109 Gravimetric

Setpoint

SF6 Error, %

of Setpoint

N2 Error, %

of Setpoint

WF6 Error, %

of Setpoint

7% 0.21% 0.28% 0.37%

13% 0.00% 0.30% 0.50%

33% -0.30% 0.02% -0.24%

67% -0.19% -0.10% -0.68%

100% -0.09% -0.65% -0.26%

€d KINETICS
The Good News

• Achieving accuracy is not magic

• Discipline, Hard Work, and Persistence

The Bad News

• Once you get your act together, can you

change the character of your product?

• What do you do when you still can't agree?

• Future processes are demanding greater range

• Current technology is at limited to 1 % SP

• Still Confusion

€rJ K I N E T I C S
The Impact of Various Gas Properties on

The Operation of an MFC

By Dan Mudd, 5/15/2000

MASS FLOW ASSOCIATES of TEXAS

VJHH Mid Rivers Mull Drive, Suite 81 17 • Sr. Charles. MO 633114 PHONE: 636-922-3670 • e-mail: dtm(«!mr'cl.i:um • FAX: 636-M1-688I

Presentation Outline

• Why Gas Properties Are of Interest

• Components of a Simple MFC and the Role of the

Various Gas Properties

• Second Tier Influences

54
Why Are The Gas Properties of Interest?

• They Suggest That the Configuration of the MFC Should

Change With The Nameplate Gas.

• Sheds Light on Surrogate Gas Calibration Procedures and

Limitations.

• Indirectly Affects MFC to MFC Variability.

Corrponents of a Sirrple fVFC and the Role of

Various Gas Properties

Maintain the Split Ratio Slay in the LinearRegion orMatch NonLineanties

-Sensor: Thermal Cond uc liv ily . Kl

(ot Gas and Air) Specific Heat. Cp

Density @ STP ,P S ensor Design

Flow Res trie tor: V isc osity . v Density«STP.P

Hestnctor Design

^ M olecular W eight

Mass Flow Associates of Texas www.mfc1.com

55
Sensor Gain * Flow Rate, f(p, Cp & Geo) — Linearity Term = f(Kt p, Cp & Geo)

mm Theoretical Signal = m*(pCp)*Ie*(-L/m)-2e*<-L/2m)*1] x Test Data From a Thermal Sensor

[ The Linearity Factor, L. Will Scale The X Axis While The Oas Conversion Factor, pCp. Scales The Y Axis
Valve Seat Stroke Effects Due To Gas Properties

Ratio of Sensor Conversion Factor To Seat Conversion Factor Relative to Nitrogen Ratio

I -

1

i

Gas Density® STP (g/l @ 0 Oeg C)

Ratio For Individual Gases Relative To N2

|SensorCF = f(p. Cp), Seal C F = ffl/M Wffl 5)|

Gas Properties: Second Tier Influences

• Non Ideal Gas Behavior - Compressibility Factor - Virial Coefficients

• Properties of Newer Gases are Less Accurate or Not Available

• Temp and Pressure Influence Can Influence MFC in Specific Cases

57
Summary

Thermal Conductivity, Specific Heat, Viscosity, Density and

Molecular Weight are The Primary Properties Influencing MFCs.

The Gas Properties Suggest That the Configuration of the MFC Should

Change With The Nameplate Gas.

The Gas Properties Shed Light on the Surrogate Gas Calibration Procedures and Limitations.

Gas Properties Indirectly Affects MFC to MFC Variability
NIST's Program to Measure

The Thermophysical

Properties

of Semiconductor Process

Gases

John J. Hurly and Michael R. Moldover

Physical and Chemical Properties Division,

National Institute of Standards and Technology,

Gaithersburg, MD 20899-8380

John J. Hurly and Michael R. Moldover

Which Gases Studied?

Table 1. Experimental T and P ranges. T Range P Range No.

(K) (MPa) Points

CF4 300 < T < 475 0.10 < P < 1.5 114

C2F6 175 < T< 475 0.10 < P < 1.5 181

SF6 230 < T< 460 0.10 < P < 1.5 280

BCI3 300 < T < 460 0.05 < P < 0.15 119

HBr 230 < T < 440 0.05 < P < 1.5 232

Cl2 260 < T < 440 0.10 < P< 1.5 326

WF6 290 < T < 420 0.05 < P < 0.3 146

(CH2 ) 20 285 < T < 420 0.05 < P < 1.0 339

,v,lcrr

John J. Hurly and Michael R. Moldover
Sound

Source

Diaphragm

Flange

Microphone

Detector

Wave

Guide

Screen

.Gold O-Ring

Diaphragm

Bottom

'late

Sound Speed.

Ideal-Gas Heat-Capacity, CP°(7).

P(T,V), Equation of State.

Thermal and viscous losses at the boundaries.

Duct effects

Cylindrical Resonator

Nisr ma BBBBBBBBHBiBBH

John J. Hurly and Michael R. Moldover

Analysis of Sound Speeds.

260

240

220

200 -

Chlorine

0-o-oa 420K

^£90, \ 1 0.0

Nisr

60

0.5 1.0 Pressure (MPa)

1.5

Acoustic Virial Equation Of State

„2_ y°RT Bp y p

2 S p

3

1 + ILL + 1LL_ + _i_L + . m \ RT RT RT

• Zero-Pressure intercept - CP°(J)

C°P (T) yQ (T)/M

J

R y0 (T)/M-\

Slope - P(T,V)

John J. Hurly and Michael R. Moldover
Ideal-Gas Heat-Capacities

140

.2T 120

« 100

60

S F 6

200 300 400 Tem peralure (K)

500

Figure 3. Measured Ideal-Gas Heat-Capacities for SF6 compared to various calculated values from spectroscopy.

imist.

John J. Hurly and Michael R. Moldover

Virial Equation of State

P = R Tp \ 1 + B(T)p + C(T)p 2

+ •

•

• Exact Thermodynamic Relations Relating

Acoustic to Density Virial Equation of State.

Algebraic expressions for B{T), C(T)

Able to Fit u(P,T) Surface.

Nisr

John J. Hurly and Michael R. Moldover

61
Hard-Core Square-Well Model

= bo

[ 1 - ( X

3 - 1 ) A ] V«

j C(7) = 1^(5- c

t A - c

2 A

2 -c3 A3

) 8

1 :

i e ;

'

J i

? c, = A.6 - 18 A.4 + 32 A. 3 - 15

c

2 = 2 A

6 - 36 X

4 + 32 X

3 + 18 X2 - 16

c

3 - 6 A

6 - 18 X

4 + 18 X

2 - 6

-a-H Aa^

where A =exp (e/k^T) -1, e is the well depth,

A is the ratio of the attractive diameter to a hard diameter,

b0 = 2/37iNAa

3 is the molar volume of the hard core. MICT

John J. Hurly and Michael R. Moldover

Fitted SF6 Sound Speeds

0.01

0.00

•0.01 -

0.5 1.0

P ressure (M Pa)

Deviations of SF6 speed-ofsound data from fitted

equations,

[( "exp "^eos ) / "eos 1 X 10°- Key: 460K; • 440K;

420K; T 400K; 380K; • 360K; + 340K; 320K;

O 300K; A 280K; V 270K;

O260K; O 250K; * 240K;

X 230K.

Nisr

62

John J. Hurly and Michael R. Moldover
Virial Coefficients of CF4

10 00 0

5 000 -

CFi

, Experimental

1 Temperature Range

NISi

200 400 600 800 Tern perature (K)

Virial Coefficients of CF4

Key: fit to the HCSW

) fit to the HCLJ.

Data: • Ref. [11];

Ref. [12]; A Ref. [13];

T Ref. [14]; Ref. [15];

O Ref. [16]; Ref. [17];

A Ref. [18]; V Ref. [19].

John J. Hurly and Michael R. Moldover

Advanced Modeling

Hard-Core Lennard-Jones 12-6 Potential.

cp(r..) = 4 e

Axilrod-Teller triple-dipole term

v

123 ( 1 + cos 9 j cos 0

2 cos 93 )

( o ^

12 ( O

!

a - 2a a - 2a

r.. - 2a r.. - 2a

K U J V y J

( P( r

l23> =

3 3 3 r

l2 rl3 r23

Nisr

John J. Hurly and Michael R. Moldover

63
Fitted HBr Sound Speeds

o

x 0.00

<i

•0.01 -

500 1000 Pressure (kPa)1500

Deviations of measured sound

speeds in HBr from fitted

equations,

[( "exp ) / ] X 100.

Key: • 230 K; 240 K;

250 K; T 260 K; 280 K;

O 300 K; 320 K; A 340 K:

V 360 K; O 380 K; • 400 K;

X 420 K; + 440K.

Nisr

John J. Hurly and Michael R. Moldover

Estimated Viscosities

Gas viscosities. Curves and

Open symbols are estimates;

Solid Symbols are measurements.

Key: present estimate;

HBr: Ref. [25]; A Ref. [26];

BC13: V Ref [30];

SF6: O Ref. [27]; Ref. [28];

Ref. [29]; T Ref. [30].

Eucken Approximation.

200 400 600 800 1000

Tern perature (K)

L J Eucken ' ^ 15 R 5 ) Nisr

_64

John J. Hurly and Michael R. Moldover
Fill Duct

Diaphragm Central Disk Shell

nist

Greenspan Viscometer

John J. Hurly and Michael R. Moldover

nist

0.5

0.0

O

o

-1.0

0.5

0.0

Before Calibration

t

• 4.

T

• • —T

• • • I v • o m ° V

• •

2 ; o n A"

<* O

o i

A

0 1

1 P/MPa 2

S. -0.5 -

-1.0

<9 •

oK

o

After Calibration

Ar 25'-C A CH„ 25=C T Ar 75'C V CH,, 75"C

He, 25 C O Nj. 25-C

He. 75 C • Xe. 25°C

PI MPa

John J. Hurly and Michael R. Moldover
Nisr

Prandtl Number Device

(Pr ^ r)QX)

John J. Hurly and Michael R. Moldover

TM 0.05

ii

1

A m n o o

_i i i i_ S,/rh or ^/rh

0»s 12 3 4 5 arooo O O A

xenon • * t A v O

^rffc- 8« B 5 0

i i i

<J„/r„ or 4 /rn

Nisr

66

John J. Hurly and Michael R. Moldover
Tungsten Hexafluoride

M.W. (1 ] 297.84

N.B.P. (2] 290.25 K

T.P (2] 275.0 K WF6

ft [3] 4.57 MPa npi

452.7 K

V.P]

0.1 mVkmol

r

C^(T\IR Vapor

Pressure MPa

sen

cm'-mol'1 &BI&TTcrrr'mor 1 cm

cm'-mol'1 dC/dTTcm'-mol 2 K mw/(m

K)

1 uPas

Estimated

Uncertaini

y

1.0/0.1% 1% Gas densities are calculated to better than 0. 1 %

ovtr the temperature and pressure ranges of the

reference.

10% 10%

Refererce [41/(51 [61 [51 [51 [51 [51 [51 [51 255 13.49 15.47 -1097.3 2819.0 -505611 5435305 6.5 16.05 260 13.60 21.22 -1044.2 2654.8 -409306 4512569 66 16.28 265 13 71 28.66 -995.0 2505.4 -330733 3760214 6.8 16.51 270 13 82 38.15 -949.5 2369.0 -266380 3143590 6.9 16.75 275 13.92 50.09 -907 2 2244.1 -213492 2635750 7.1 16.98 2S0 14.03 64.94 -867.8 2129.6 -169892 2215514 7.3 17 21 :s5 14 13 S3 :: -831.1 2024.3 -133851 1866498 7.4 17.44 290 14.23 105.45 -796.7 1927.2 .;:<*«» 1575285 7.6 17.67 295 14 33 -764.5 1837.5 -79201 1331447 7.7 17.91 300 14.42 -734.4 1754.5 -58589 1126565 7.9 18.14 References:

1. IUPAC "Aiomic Weights of the Elements 1993';/ Phys. Chem. Ref. Data 1995. 24. 1561.

2. E. F. Westrum. Pure and Appl Chem., 1964. 8. 1 87. 3. V. V. Malyshev. Tepiofizjka Vysoldkh Temperaiw. 1973. 1 1. 1010.

4. M. W. Chase. "NIST-JANAF Themocbemkal Tables. Fourth Edition', J. Phys. Chem. Ref. Data, Monograph 9. 1998. 1-1951.

5. J. J. Hurly. "Thermophysical Properties of Gaseous Tungsten Hexafluoride from Spced-of- Sound

Measurements

-

. Int. J. Thermophys. . In Press.

6. D. R_ StulL "Vapor Pressure of Pure Substances", Ind £n? Chem. 1947, 39, 517.

Figure 9. Example Web Page for the On-Line Semiconductor Process Gas Properties Database. * l,gr

John J. Hurly and Michael R. Moldover

Index of Semiconductor Process Gases

Argon Ar Nitrogen Tri fluoride NF3

Allene CFU Nitrogen Hi

Arsenic Tri fluoride AsFj Phosgene COCl 2

Arsine AsH, Phosphourous Trifluoride PF,

Trimethyl Arsine As(CH,), Phosphorous Pentafluoride PF,

Diborane B2 H Phosphine PH,

Pentaborane B<Hv Sulfur Dioxide so.

Roron Trichloride B£ Stibi ne SbH,

Bromine Br Silane SiH,

Carbon Monoxide £Q Disilane Si 2 H6 Carbon Tprrafliinride C& Silicon Tetrachloride SiCl,

Chlorine £k Silicon Teterafluonde SiF,

Chlori ne Tri fl uori de OF, .Snlfir Hexafluoride SEi

Ethylene Oxide C2 FL,0 Titanium Tetrachlofirde TiCU

Helium He Tungsten He.xaflnnndp 2£Ei

Hexafluroethane C,F« Uranium Hexafluoride UF6

Hydrogen Bromide HBr Vinyl Bromide C2 H,Br

Hydrogen Chloride HO Vinyl Fluoride QH,F

Hydrogen Fluoride HF Vinyl Chloride c2 h3 ci

Hydrogen Sulfide H2 S Trimethyl Gallium Ga(CHj)j Molybdenum Hexafluooride MoF6 Triethyl Gallium Ga(C2 H5)3

Nitric Oxide NO Trimethyl Indium In(C2H5)3

Nitrous Oxide NO.

John J. Hurly and Michael R. Moldover
Conclusions

We can measure sound speeds ur < 0.01% in process and

surrogate gases spanning the ranges

0.05 < P < 1.5 MPa and 200 < T<475 K.

From Sound Speeds we deduce the ideal-gas heatcapacity, and the virial equation of state which is valid

outside our experimental temperature range. uT < 0.1%

Through advanced modeling, we can estimate transport

properties over a wide temperature range. ur < 10%

We are developing advanced acoustical techniques for

measuring viscosity and thermal conductivity.

We will make the results available in a user friendly

format, via web or PC program.

NisrJohn J. Hurly and Michael R. Moldover

68
cure processing

Flow Controller fa Semioonducta

ndustry

Ka/ehZcrkcr Ph.D.

Manager, Ach/anced T echndogy

NIST

Ma/ 1 5- 1 6- 00

Microelectronics Division

"...reductions in feature size end inaecses in wafer

dameter ere not s uffident to keep the indus try on

its historic 25-30% rrxr^ufecturing cost learning

curve.

. . i mcrovements i n devel op ng purches i ng and

operating equipment ere required. . .OE E

.
pure processing.

• Semioonducta Key Industry trends.

• Key Processes.

8 Dynamics.

• Technology develocrment trends.

• Technicd Trend fa Mcbs Flow Contrd.

Microelectronics Division RE

pure processing.

• Nationd T echndog/ R ocarrp fa S emconductas

1999 2000-2002 2003 TREND CATEGORY: TREND TREND IMPLICATION TREND

M in Feature Size 250nm 180 - 150 nm New materials

are needed.

130 nm

DRAM Level 65 Mb 256 Mb- 1G Material QC 4G Number ot metal levels (Logic) 6 6-7 7 Interconnect M etal Al-Cu A1-Cu Cu

IMD Si0 2 Si02 , SiOF

SiOF, Aerogels,

etc. Gate Oxide 40-45A 35-40A 20-30A

Contact / via CD 0.28 0,2 N/A

Contact via aspect ratio (Logic) (DRAM) 5.5:1 6.3:1

Amorphous

Carbon for Ultra Low K,

Microelectronics Division MILLIPORI
cure processing

• Shift in the Industry trend from Batch Process to

S incje Wafer would impact the tradtiond Gas

S ys tern Components

.

- Low Flow Rates for some processes <1 seem, etch

CVD processes

- Higher flow rates fa RTP. EPI ( 100-300slm)

- Low Pressure Drops

- ES C Adoption for Vacuum Processes

- Heat T rensfer end Pressure Control of Wafer on the

Chuck. (Backside Wafer Coding/ Heating)

- Integration of cndylicd tods with eouipment

Mil 1 1PORF

Macdectrcnics Division lYllLUr WI\L.

f J 1 f 1 I I 1 1 I ^ I Dure procaine

• Improve OEE ( MTBF.MTTR). under new

perfamence requirement.

• Automation/ unifam communioation protocol.

• New fvlaterids handing/ process.

• Red Time Process Contrd.

• Tod Cost/ Footprint Reduction.

• Sofety/Environmentd.

• Process Intecjation.

• Lower Qxisunncde oost per de.

MILLIPORE ; Mcreeledrcnics Division
list HE

Dure process no

• Mi gati on to Lower Process Pressure HDCVD

I • Mi gati on to Li quid Source P re-curs as (SACVD)

I • Low end High K Dielectric materid acK/cncement

f • Higher Process Temperature red pes.

I • IrvChcnioer Gos Monitoring end Delivery Control

j • Direct Liquid Injection, Vcporizer systems

!

• Backside Wafer Cooling/ Heating

I Miaoeledrcnics Division
S ACVD (TEOS/ 03), w'll be the man techndog/

focus for encaps uiation of S OD end capping la/ers

fa the next few generations

- TEOS is themaferid of the choice fa FEOL prooesses

- Liquid/ bulk precursors aeemergngeppficatiens

- DLI, Chdlenges fa Liquid Source delivery

Requirement:

- Liquid MFCs fa DLI

- Vcpaiza systems

- RctxjstPlatfamtechndogy fa liquid/vcpa delivay

Maodecfrcnics Division MILLIPORI

pure processing

• Low end High K materids aeacK/cndng.

M a t e r i a I m iN f

iO 2 EiO F P o I y a m i d e Hydrogen- Silsesquioxane HSQ

Ifluorinated Polyam ides M ethyl Silsesquioxane M SQ

Organic Polymers

Polyarylene Ethers

P a r y I e n e F Fluorinated Amorphous Carbon

T e f I o n

Silica Aerogels

.Air Bridges

Maoelectronics Division

Value D e p o s i t i o n M e t h o d

7 CVD

4 CVD

3 .3 CVD

3 -3 .5 S p i n - o n

3 S p i n - o n

2 .8 S p i n - o n 2.7. S p i n - o n

2 .3 -2 .7 S p in -o n

2 .6 S p i n - o n 2 .3 CVD

2 .2 CVD

2.1 C V D , S p in - o n 1.1-2.0 S p i n - o n

1 .0 Subtractive

MILLIP

73
• Dielectric oontinued

- Most necr future schemes involve vopaized liquids - Most liquids ere dr reactive- Ccrrier gas purity ccntrd end

better delivery systems ae needed

Requirement

- Bulk HCL purification fa charter decn is ided. Hic^i oapadty purifiers ae needed.

- Higfi Flowoontrdlers fa HCL &NH3. Snrdl aap'llay MFCs

ae not suited Lage Ccpillay end P-based should be

considered

- Low inlet pressure MFCs fa SSD* cpdioation.

*S S D = S did S ource Delivery

Microelectronics Division MILLIPORE ,T

., "'T I w *

Direct Liquid Injection, Vcpaizer Systems.

- Materid prcperties ddcrteprcdudtechndogy

devdopment.

Chemiod categories:

- Chemiods used in the future T echndogy T rends fa Metd

CVD, Dielectric CVD, Baria CVD, EPI enddeen ae

often dfficult to honde, due to their properties

.

• Liquid Stability

• Vcpa Stability

• Viscosity

• Toxicity

MaoeJectrcnics Division MILLIPORE
mm p Category Flow R Vapor P Stable Gas

A Low High Yes TEOS.TMP

TiCI4,TDMAT

B Low Low Yes Ta205.TDEAT

TEASAT

C Med High No Cu(l),TaN

D Low High Yes (Pyro) DMAH

E High High Yes(Corr) HSiCI3,TiCI4,

H2SiCI2

F Low Low No (solid) BST.PLZT, SBT

G Low Low Yes (Toxic) PH3,AsH3,BF3

Microelecfrcnics Division MILLIPORE

r oore processing

Requirement:

- l[>Chcrnber Gcb Constituency Mcnitaing systems

- DevioeNetcs Sens a Bus aime mover.

- Network reed/ Gcs Pcnet cxrnponents.

- Self dccnc6ticccpctility (Interactive Sens as) is Key.

- Multifunctiond oomponents ( Filters /Purifiers, MFCs) is required fa the ccs t aid "footprint" reduction.

Maoelectrcnics Division MILLIPORE

75
Dure- process Transducers

Isolation Valves

Filters/Purifiers

CDG's

Setpoint from Tool"

Microelectronics Division MILL1POI

pyre processing

Mess F low Controller Techndog/.

- Thernnd Mass Flow Controllers

- P- Bos ed Moss Flow Controllers

- Sonic Nozzle Moss Flow Controllers - MEMS bosedMcss Flow Controllers - Coridis bosedMcss Flow Controllers

- Acoustic Flow Controllers

Future MFC Perfamcnce. (Key Attributes)

- Mechcnicd Design ( Vdve, FlowSensors)

- E lectronic Des ign ( Andog. Dig'td) - Ser^cecfcility/Rdicfcility (Self Dicgnos tics) - Cornmunications (Sensa Bus motivation)

Microelectronics Division

76
All Mess Flow Controllers, hove in common,

three functiond elements:

- "Sensor" to measure the Moss Flow Rate.

- Vdve" to regulate the flow of gas.

- Electronics "to trans I cite inputooiTYTxrios to

achieve the des ired flow rate output.

McroelectTcnics Division MILLIPORE

77
sure processing.

Flow Splitter

Flow Sens a

Control Vdve

Electronics

Microelectronics Divisicn

Based on Flow through an Orifice

AP across orifice is proportional to the volumetric

flow rale through the onlice. Flow is considered choked when the velocity is sonic This

is considered critical How and is the maximum velocity tor a given inlet pressure. For critical llow conditions:

t ///////////////////////

r

Flow . VI. PI j| V2- P2 77777777777777777777777 /

Orifice plate

q=.01749'(P1 (fsa/29.7)-NJ MWa ,MWgas .^2 (jlm) or

q=C13.63*P1,_ Br M

]rT ~

Microelectronics Division

78
pure processing

Flow Orifice Plate.

Upstream PressureTrcnsduoer

Downs trecm P res s ure T rcns ducer

Control Vdve

Electronics

Maoelecfrcnics Division MILLIPOR!

oore processing

• B csed on mecsuring Flow throucfi cn orifice under

" Choked Condtion".

- Sonic Nozzle Orifice

- "Upstrean" Press ure T rcns ducer

- Contrd Vdve

- Electronics

Maoelectrcnics Division

79
^^^^^^^^^^^^^^^^^^

• BcBed on mecsuring Flow throu^i cn aifioe, using

"MEMS "sensors.

- Miaomachined Silicon Orifice - Mi aomachined Pressure Sens a

- Mi aonncchined Control Vdve

- Electronics

Microelectronics Division

pure procaine

I • Accuracy

l • Linecrity

I • Repeated I ity

I • Reproducibility

; • TrcnsientChaacteristics

I • Leok Integrity

I • Patide Generation

I Miaceiectrcnics Division

• Pressure Coeffi dent

• T enperature Coefrldent

• Attitude Sensitivity

• Long Term Stability

• Vdve Leok T hrough

• Reliability

• Serviceability

vMLUPORE

80
pure prccessinq

Increased Functiondity

- Improved Accuracy ( Dig'td vdve contrd) - InCTecsedDyncmicRcnge. > 100 :1 - Inaecsed Ccntrdlddlity. - Elim'nation of mechcnicd/mcnud acjustment

- Multiple Gcs curve stacge.

- E rrfcecded 'Dreg & Drop" multigcB Cdifrcri on database.

- Elimination of Overs hoot/ undershoot for fastTTS . - Self- Diagnostics to reduce Tod downtime.

• Rawsensor monitor

• Contrd Vdve Current or vdtage

• F low Os dilation

• Gcs line Pressure measurement.

• Gas Line Temperature measurement

Maoeledronics Division MILL! PORE

pure processing

Calibration o( a Mass Flow Controller with Trimethylsilane. Comparison o( different Methods



• Ccnddates

- WaldFlP

- CAN* ( DevioeNet. S DS ) - LcnWaks

- Seriplex

- ISP

- BittDus /IEEE-118

*CAN= Contrdler Area Network

Factors considered

- Interoperability

- Avdlability

- Survivability - Repeatability

- Speed

- Flexibility - Node Cost

- T rack reoora

- Determinism

- Node Size

- Tods & development Cost

Microelectronics Division MILLIPORI

pure processing

CAN based ( Contrdler Area Network) protccds will expend repdy in the next few yeas

.

DeviceNet is the front runner end is the protocd of

chdee with severd mq'a OE Ms

.

DeviceNet has famed ODVA ( Open DevioeNet

Vendor As sedation).

• Europecn PNO( ProfiBus Usa Orgcnization) andits

nath American am PT Q ae s uppated by S iemens

aid maiy E uropeon OE Ms end will be strong in

Europe.

Moroeiectronics Division MILLIPOI

85
pure processing

NewPlatfam Dig'td Mess Flow Controller would

be the heat of the Charter P rooes s Contrd

.

- Pressure Insensitive

- Multi-Gcs

- Wide DyncmicRcrige

- Peer to Peer Communication

- Distributed Control - DevioeNet end ProfiB us ore protocols of the choice.

- In-Situ Chamber Gos Constituency monitor tooontrd the

Mess FlowofGos, eventudly would reel ace the

oonventiond " Dewnstrean Pressure Contrd" techniques

.

Microelectronics Division


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