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SEMI MF1527-1104 © SEMI 2003, 2004 2 3 Referenced Standards 3.1 SEM I Standards SEMI C28 — Specifications and Guidelines fo r Hydrofluoric Acid SEMI C35 — Specifications and Guideline for Nitric Acid SEMI C39 — Specifica…

SEMI MF1527-1104 © SEMI 2003, 2004 1

SEMI MF1527-1104

GUIDE FOR APPLICATION OF CERTIFIED REFERENCE MATERIALS

AND REFERENCE WAFERS FOR CALIBRATION AND CONTROL OF

INSTRUMENTS FOR MEASURING RESISTIVITY OF SILICON

This guide was technically approved by the Global Silicon Wafer Committee and is the direct responsibility

of the North American Silicon Wafer Committee. Current edition approved for publication by the North

American Regional Standards Committee on August 16, 2004. Initially available at www.semi.org

September 2004; to be published November 2004. Original edition published by ASTM International as

ASTM F 1527-94. Last previous edition SEMI MF1527-02.

1 Purpose

1.1 Resistivity is a widely used parameter for

specification and characterization of silicon wafers for

use in fabricating semiconductor devices and integrated

circuits. Many types of instrumentation used for

making resistivity measurements including the non-

contact eddy-current instruments used for

measurements made in accordance with SEMI MF673,

DIN 50445, or DIN 50447 require calibration because

they are relative measurements. Although

measurements made with in-line four-point probes in

accordance with SEMI MF84 or DIN 50441 are, in

principle, absolute, control charts should be maintained

for four-point probes because one cannot always be

sure that the electrical resistivity of the test specimen is

sufficiently homogeneous for the theoretical model of

the method to apply, that the electrical thickness of the

wafer is exactly equal to its measured mechanical

thickness, or that the stability of the instrument is

adequate.

1.2 Instruments for measuring such related parameters

as spreading resistance (used in accordance with SEMI

MF525 or SEMI MF672), net carrier density (used in

accordance with SEMI MF1392, SEMI MF1393, or

DIN 50439), and sheet resistance (used in accordance

with SEMI MF1529) also require calibration.

1.3 For all these purposes, wafers of known resistivity

are required. Such wafers are supplied by several

sources with a wide range of certified or calibrated

resistivity values. Although these wafers are often used

directly, the resistivity values represented by purchased

standards can also be transferred to an in-house

resistivity reference wafer that is then used for routine

instrument calibration or control.

1.4 The accuracy with which this transfer can be

affected depends not only on the procedures for using

such reference wafers but also on the procedures for

material selection, instrument qualification, and

calibration of the reference wafer. This guide provides

recommendations for procedures for these operations

appropriate to obtaining the best available accuracy in

use of resistivity reference wafers.

1.5 These procedures are specifically intended for use

in measuring the resistivity of silicon wafers.

Extension to resistivity measurements on other

semiconductor materials or to resistivity values outside

the range covered by the resistivity reference wafers has

not been demonstrated.

2 Scope

2.1 This guide covers the application of Certified

Reference Materials (CRMs) for resistivity

measurements on silicon wafers. Specifically, this

guide covers the use of these CRMs for preparing

resistivity reference wafers and for ensuring the quality

of the instrumentation used for preparing them.

2.2 The guide covers the selection of materials for

resistivity reference wafers, procedures for preparing

and calibrating resistivity reference wafers, and use of

resistivity reference wafers in qualifying, calibrating,

and controlling various types of resistivity

instrumentation.

2.3 The guide provides criteria for selection of

instruments for determining the resistivity of silicon

resistivity reference materials, procedures for

maintaining such instruments in statistical quality

control, and training requirements for operators

engaged in making and using resistivity reference

wafers.

2.4 Related Information is included that covers (1)

suggested control charting procedures for organizations

that do not already have such procedures in place, and

(2) errors in resistivity determination that result from

uncertainties in wafer diameter, wafer thickness, and

probe-tip spacing.

NOTICE: This standard does not purport to address

safety issues, if any, associated with its use. It is the

responsibility of the user of this standard to establish

appropriate safety and health practices and determine

the applicability of regulatory or other limitations prior

to use.

SEMI MF1527-1104 © SEMI 2003, 2004 2

3 Referenced Standards

3.1 SEMI Standards

SEMI C28 — Specifications and Guidelines for

Hydrofluoric Acid

SEMI C35 — Specifications and Guideline for Nitric

Acid

SEMI C39 — Specification for Potassium Hydroxide

Pellets

SEMI M1 — Specifications for Polished

Monocrystalline Silicon Wafers

SEMI MF43 — Test Methods for Resistivity of

Semiconductor Materials

SEMI MF81 — Test Method for Measuring Radial

Resistivity Variation on Silicon Wafers

SEMI MF84 — Test Method for Measuring Resistivity

of Silicon Wafers with an In-line Four-point Probe

SEMI MF525 — Test Method for Measuring

Resistivity of Silicon Wafers Using a Spreading

Resistance Probe

SEMI MF533 — Test Method for Thickness and

Thickness Variation of Silicon Slices

SEMI MF672 — Test Method for Measuring

Resistivity Profile Perpendicular to the Surface of a

Silicon Wafer Using a Spreading Resistance Probe

SEMI MF673 — Test Method for Measuring

Resistivity of Semiconductor Slices or Sheet Resistance

of Semiconductor Films with a Non-contact Eddy-

current Gage

SEMI MF723 — Practice for Conversion Between

Resistivity and Dopant Density for Boron-doped,

Phosphorus-doped, and Arsenic-doped Silicon

SEMI MF1241 — Terminology of Silicon Technology

SEMI MF1392 — Test Method for Determining Net

Carrier Density Profiles in Silicon Wafers by

Capacitance-voltage Measurements with a Mercury

Probe

SEMI MF1393 — Test Method for Determining Net

Carrier Density in Silicon Wafers by Miller Feedback

Profiler Measurements with a Mercury Probe

SEMI MF1529 — Test Method for Sheet Resistance

Uniformity Evaluation by in-line Four-point Probe with

the Dual-configuration Procedure

SEMI MF1530 — Test Method for Measuring Flatness,

Thickness, and Thickness Variation on Silicon Wafers

by Automated Non-contact Scanning

SEMI MF1618 — Practice for Determining Uniformity

of Thin Films on Silicon Wafers

SEMI MF2074 — Guide for Measuring Diameter of

Silicon and Other Semiconductor Wafers

3.2 ASTM Standard

D 5127 — Guide for Ultra Pure Water Used in the

Electronics and Semiconductor Industry

3.3 DIN Standards

50431 — Measurement of the Electrical Resistivity of

Silicon or Germanium Single Crystals by Means of the

Four-Point-Probe Direct Current Method with Collinear

Four-probe Array

50439 — Determination of the Dopant Concentration

Profile of Single Crystalline Semiconductor Material by

Means of the Capacitance-voltage Method and Mercury

Contact

50445 — Contactless Determination of the Electrical

Resistivity of Semiconductor Wafers with the Eddy

Current Method

50447 — Contactless Measurement of Electrical

Surface Resistivity of Semiconductor Layers by Eddy-

current Method

3.4 ISO Standards

Guide 30:1981 Terms and Definitions Used in

Connection with Reference Materials

ISO 8402 — Quality—Vocabulary

ISO 10012-1 — Quality Assurance Requirements for

Measuring Equipment—Part 1: Management of

Measuring Equipment

NOTICE: Unless otherwise indicated, all documents

cited shall be the latest published versions.

4 Terminology

4.1 Definitions Terms Related to Reference Materials

4.1.1 certified reference material (CRM) — a reference

material one or more of whose property values are

certified by a technically valid procedure, accompanied

by or traceable to a certificate or other documentation

1 Annual Book of ASTM Standards, Vol 11.01, ASTM International,

100 Barr Harbor Drive, West Conshohocken, PA 19428. Telephone:

610-832-9500, Fax: 610-832-9555, Website:

www.astm.org.

2 Available in both German and English editions from Deutches

Institut für Normung e.V., Beuth Verlag GmbH, Burggrafenstrasse 4-

10, D 10787 Berlin, Germany, website:

www.din.de.

3 ISO Central Secretariat, C. P. 56, CH-1211 Genève 20,

Switzerland, Website:

www.iso.ch, available in the U.S. from

American National Standards Institute, 11 West 42nd Street, 13th

Floor, New York, NY 10036, Website:

www.ansi.org

SEMI MF1527-1104 © SEMI 2003, 2004 3

which is issued by a certifying body (ISO

Guide 30:1981).

4.1.2 Discussion — ISO 8402 states that in a

calibration sense, traceability relates measuring

equipment to national or international standards,

primary standards, or basic physical constants or

properties. In the present guide, as in ISO 10012-1, the

term “measuring equipment” is extended to include

both measuring instruments and measurement standards

(including reference wafers).

4.1.3 reference material (RM) — a material or

substance one or more properties of which are

sufficiently well established to be used for the

calibration of an apparatus, (for) the assessment of a

measurement method, or for assigning values to

materials (ISO Guide 30:1981; ISO 10012-1).

4.1.4 resistivity reference wafer — a CRM or RM in

the form of a silicon wafer or chip used for routine

calibration or control of resistivity measuring

equipment.

4.1.5 Standard Reference Material (SRM

®) — a

certified reference material issued by the U.S. National

Institute of Standards and Technology.

4.1.6 traceability — the ability to trace the history,

application, or location of an item or activity, or similar

items or activities, by means of recorded identification

(ISO 8402).

4.2 Definitions of Terms Related to Four-point Probes

4.2.1 four-point probe — an electrical probe

arrangement for determining the resistivity of a material

in which separate pairs of contacts are used (1) for

passing current through the specimen, and (2)

measuring the potential drop caused by the current.

4.2.2 probe head, of a four-point probe — the

mounting that (1) fixes the positions of the four pins of

the probe in a specific pattern such as an in-line

(collinear) or square array, and (2) contains the pin

bearings and springs or other means for applying a load

to the probe pins.

4.2.3 probe pin, of a four-point probe — one of the

four needles supporting the probe tips; mounted in a

bearing contained in the probe head and loaded by a

spring or dead weight.

4.2.4 probe tip, of a four-point probe — the part of the

pin that contacts the wafer.

4.2.5 probe-tip spacing, of a four-point probe — the

distance between adjacent probe tips.

SRM

is a registered trademark of the U.S. National Institute of

Standards and Technology and the U.S. Government.

4.3 For definitions of other terms used in silicon wafer

technology refer to SEMI M1 and SEMI MF1241.

5 Reagents

5.1 Purity of Reagents — All chemicals for which such

specifications exist shall conform to Grade 1 SEMI

specifications for those specific chemicals. Other

grades may be used, provided it is first determined that

the chemical is of sufficiently high purity to permit its

use without lessening the accuracy of the test.

5.2 Purity of Water — Reference to water shall be

understood to mean water meeting the requirements of

Type E-3 water or better as described in ASTM Guide

D 5127.

5.3 The recommended chemicals shall have the

following nominal assays:

5.3.1 Nitric Acid, HNO

, concentrated, 70 to 71%,

Grade 1 in accordance with SEMI C35,

5.3.2 Hydrofluoric Acid, HF, concentrated, 49.00 ±

0.25%, Grade 1 in accordance with SEMI C28, and

5.3.3 Potassium Hydroxide, KOH, pellets, 85% min,

Grade 1 in accordance with SEMI C39.

5.4 KOH Etching Solution — Dissolve potassium

hydroxide (KOH) in water to make a 50 weight % KOH

solution in sufficient volume to allow complete

immersion of the largest wafers to be prepared for test.

This solution is to be used at a temperature of 65 to

75°C.

5.5 Etching Solution (15 + 1) — Mix 15 parts of nitric

acid (HNO

) with one part of hydrofluoric acid (HF) in

sufficient volume to allow complete immersion of the

largest wafers to be prepared for test.

6 Resistivity CRMs

6.1 Resistivity CRMs are available from several

sources in a variety of configurations, orientations,

conductivity types, and resistivity. Choose the

configuration to match the desired application as

closely as possible. For example, choose whole wafers

for applications involving whole wafer measurements

and chip sets with relatively closely spaced resistivity

values and appropriate orientation and conductivity

type for applications involving spreading resistance.

7 Control of Primary Resistivity Measuring

Instruments

7.1 “Primary” resistivity measuring instruments are

four-point probes used for calibrating resistivity

reference wafers. Such instruments must (1) meet the

requirements of SEMI MF84, (2) be maintained in a

state of control through the use of

and s instrument