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Vacuum Systems Cookbook

Chapter 1: Basic Skills

Chapter 2: Safety

Chapter 3: Review of Basic Vacuum Calculations

Chapter 4: Vacuum System Components

Chapter 5: Sub-atmospheric Total Pressure Gauges

Chapter 6: Mechanical Vacuum Pumps

Chapter 7: Oil Vapor Diffusion Pumps

Chapter 8: Cryo-sorption pumps

Chapter 9: Sputter ion pumps

Chapter 10: Turbomolecular Pumps

Chapter 11: Cryogenic Vacuum Pumps

Chapter 12: Leak Detection

Chapter 13: Partial Pressure Analysis

Chapter 14: Thin Film Deposition Processes

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Chapter 1: Basic Skills

Vacuum Technology 60A & 60B

In this chapter we hope to present a review of basic skills in the areas of mathematics, unit conversions, use of the metric system, an introduction to the physical nature of matter, measurement techniques, and techniques for the presentation of data. At the end of each section we will include a bibliography for those of you wishing to explore any of these areas more fully.

REVIEW of MATHEMATICS

Physical measurements you will perform will require accurate recording, calculation, and reporting of numbers. Numbers that we will use may be broken down into three categories: integers, real numbers, and rational numbers. We will use the symbols x, / or ÷, +, and - to denote the mathematical functions multiply, divide, add, and subtract.

Integers: whole numbers, either positive or negative Example: 3, -7, 1,000,000

Real Numbers: also called decimal numbers Example: 5.4, 0.001, -12.34

Rational Numbers: numbers expressed as a ratio of two numbers Example: 2/3, 1/10 and -1/2.

Mathematical Operators: addition (+), subtraction (-), multiplication (x), division(÷ )

Equations: Just as the name suggests, equations are mathematical statements in which the equality of two statements is expressed:

Example: π x 5 = 15.7 is a mathematical equation which reads Pi multiplied by five is equal to fifteen point seven (or fifteen and seven tenths).

Variables: Often we do not know the values for all of the expressions in an equation, so we substitute letters or symbols in place of the numbers. Variables are also used in the writing of generic equations (formulas) into which numbers are substituted later. Example: the circumference of a circle C having diameter D is given by the equation:

circumference = π x D or C =π D

In this example, D is a variable and can have any positive value. When variable are not separated by an operator, it is assumed to be multiplication.

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Formulas: Formulas are mathematical equations that have been worked out for you; all that is required to solve a formula is to substitute appropriate numerical values in place of the variables.

Example: the mass flow rate of a vacuum system is given by the formula:

Q = S x P

Where Q= mass flow in Torr- liters per second, S= volumetric flow rate (or pumping speed) in liters per second, and P = pressure, expressed in Torr. Formulas used in simple vacuum calculations are given in appendix X, and formulas for areas and volumes of simple geometric shapes are given in the appendix Y.

Exponential Notation: Often in the process of performing calculations, we are interested in multiplying a number by itself several times.

Example: The area of a circle is equal to a constant (π) times the square of the radius (the radius multiplied by itself). In this example, one could write the square of the radius as: r x r, but it is more frequently written as r 2 . Here, r is the base and 2 is the called the exponent.

base exponent

 Number as a power of 10 Number multiplied as often as the exponent indicates Number, N 5 4 = 5 x 5 x 5 x 5 = 625 2 3 = 2 x 2 x 2 = 8 10 6= 10 x 10 x 10 x 10 x 10 x 10 = 1000000 3 2= 3 x 3 = 9 4 3 = 4 x 4 x 4 = 64 7 1 7 7

Exponents can be negative and/or real numbers; here are some examples:

 25 0.5 = √25 = 5 2 -3 = 1/(2 3 ) 1/8= 0.125 125 1/3= 3 √125 = 5 100 -1/2= 1/(100 1/2 )= 1/10 = 0.1 4.5 -3.7 = 3.7 √4.5= 260 7 -1 1/7 0.14

Sample Problems:

1.1 Evaluate the following exponents: 2 5 , 10 3 , 56 0 .

1.2 Evaluate the following exponents: 4 0.5 , 10 -4 , 625 1/4

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MATHEMATICAL OPERATIONS with EXPONENTS:

Addition of Numbers Expressed in Exponential Notation: In order to add numbers such as 4 3 and 3 6 it will be necessary to find the value of each and then add in the usual manner. Examples:

4 3= 4x4x4 = 64 3 6 = 3x3x3x3x3x3 = 729 4 3 + 3 6 = 64 + 729 = 793

Subtraction of Numbers Expressed in Exponential Notation: Same as for addition; evaluate each exponent, then subtract.

Multiplication of numbers expressed in exponential notation: Now things really get to be interesting! Numbers expressed in exponential notation that have the same base may be multiplied by simply adding the exponent.

Example: 2 4 x 2 5 = 2 (4 + 5) = 2 9

Division of Numbers Expressed in Exponential Notation: In a manner similar to multiplication of values expressed in exponential notation, division of numbers having the same base may be accomplished by subtracting the exponents.

4

5

÷

4

3

=

4

(5 3)

4

2

==

16

What about any number raised to the zero power (a zero exponent)? Examples:

3 0 = 1 76 0 = 1

Rule: Any number raised to the zero power is equal to 1.

In all of the examples above both the base and the exponent are integers. It is possible that either or both could be real numbers (see the table below). Examples:

5.3 4 = 5.3 x 5.3 x 5.3 x 5.3 = 789 6 2.8 = 6 multiplied by itself 2.8 times = 151

Scientific Notation: Writing and calculating with very large or very small numbers can result in a great deal of tedium and often create opportunities for mathematical errors. One can express all real numbers in terms of a number between 1 and 10, multiplied by 10, and raised to some power.

Examples:

Number, N

Number multiplied or divided by 10 5.67 x 10 x 10 x 10 x 10 x 10 =

Scientific Notation 5.67 x 10 5

567000=

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 0.00034= 3.4 ÷ 10 ÷ 10 ÷ 10 ÷ 10 = 3.4 x 10 -4 1090000 1.09 x 10 x 10 x 10 x 10 x 10 x 10 = 1.09 x 10 6 354 3.54 x 10 x 10 = 3.54 x 10 2 0.067 6.7 ÷ 10 ÷ 10 = 6.7 x 10 -2 7690 7.69 x 10 x 10 x 10 7.69 x 10 3

Converting from Scientific Notation: Occasionally you may wish to change a number expressed in scientific notation back to the normal form of expression. This is accomplished by moving the decimal point to the right the number of times expressed in the power of 10 for positive exponents and similarly moving the decimal point left for negative powers of 10. Examples:

5.67 x 10 3 = 5670 3.40 x 10 -4 = 0.00034

Addition of Numbers Expressed in Scientific Notation: In order to add numbers

expressed in scientific notation, one must first make the power of 10 for each of the numbers to be added equal.

Example:

2 x 10 3 + 5 x10 5 = 0.02 x10 5 + 5 x10 5 = 5.02 x10 5

Subtraction of Numbers Expressed in Scientific Notation: Just as for addition of

numbers expressed in scientific notation, the first operation is to move decimal places to make all powers of 10 equal.

Example: 3 x10 5 -

2 x10 4 = 3 x10 5 - 0.2 x10 5 = 2.8 x10 5

Multiplication of Numbers Expressed in Scientific Notation: To multiply numbers expressed in scientific notation, the following rules are used:

(Ax10 x ) x (B x10 y ) = (AxB) x 10 (x+y)

Example:

(4 x 10 4 ) x (7 x10 3 ) = (4 x 7) x 10 (4+3) = 28 x 10 7 = 2.8 x 10 8

Division of Numbers Expressed in Scientific Notation: The rules are similar to multiplication.

Example:

(8 x 10 4 ) ÷ (2 x 10 3 ) = (8 ÷ 2) x 10 (4-3) = 4 x 10 1 = 40

Rounding of Data and Significant Figures: A measurement was made of the length and diameter of a tube in order to calculate its volume. The diameter was measured to be 4.05 cm and its length was 83.7 cm. The geometric volume of the tube may be calculated using the formula

V

2

=π rl

where V is the volume of the tube, r is the radius, and L the length.

Example: V = π × (4.05 cm / 2) 2 × 83.7 cm = 343.222313 cm 3

A comment on Significant Digits

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Reporting the calculated volume as 343.222313cm 3 is not truthful, as it suggests that the volume is known to nine significant figures, when in fact the measurements are only known to three significant figures. The result should be rounded to 343. If the last figure to be dropped in a rounding operation is less than five, round down, otherwise, round up. A good practice to follow is to round the result of a calculation to the lowest number of significant figures used in the calculation of that result.

Example: If we multiply 5.03 × 6.7 the result is 33.701, but should be reported as 33, as there are only two significant digits in 6.7.

Examples:

 Number # of significant figures rounded to 2 sig. fig.'s 12.3 3 12 345.7 4 350 0.0456 3 0.046

Sample problem:

1.3 Round the following numbers to two significant figures: 23.4, 1234, 658,1.34 x 10 -5 .

Logarithms: Every positive number may be expressed as a power of 10. We can always find a number "p" such that the number N = 10 p . We call p the logarithm of N to the base 10 or the common log of N.

Alternatively, we may write p = log 10 (N) Example:

 Number, N number as power of 10 log (base 10) of N 345 = 10 2.54 2.54 0.0056 =10 -2.3 -2.3 10,800,000 =10 7.03 7.03 0.000578 =10 -3.23 -3.23 1450 =10 3.16 3.16

Notice that numbers larger than one have positive logarithms, and numbers smaller than one have negative logarithms.

Antilogarithms: For every number expressed as a power of 10 there exists an antilogarithm. Example: The antilogarithm of 10 5 is 5.

Computation Using Logarithms:

Log (MN) = Log(M) + Log(N)

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Log(M/N) = Log(M) - Log(N)

Log(M Y ) = Y x Log(M)

Fairly complex mathematical expressions may be evaluated simply using logarithms.

Log( A Z x B W ÷ C Y ) = Z x Log(A) + W x Log(B) - Y x Log(C)

Sample Problems:

1.4 Log(2 5 × 3 2 ÷4 3 )

1.5 Log(4 3 )

1.6 × 12 )

Log(56

SYSTEM of UNITS

While it is generally agreed that use of the International System of Units (SI units) is the best practice, you will soon find that the majority of people who work in vacuum technology use some non-SI units. Torr, for example, is much more frequently used in the USA than pascal (Pa) or millibar (mbar) as the unit for pressure. We have chosen to use SI units whenever possible, but to also follow the current conventions in the United States.

Table 1.1 Names and Symbols for SI Base Units

 Physical quantity Name of SI unit Symbol for SI unit length meter m mass kilogram kg time second s electric current ampere A temperature Kelvin K amount of substance mole mol

Before moving on to the derived SI units, some explanation of the base units may be appropriate.

Meter: The length of the path traveled by light in vacuum in the time interval 1/299,792,458 of a second. A meter is approximately 39.4".

Kilogram: Equal to the mass of the international kilogram prototype. The mass of an object is related to its weight by the force of gravity given by the equation weight = mass x gravity. A kilogram is about 2.2 pounds.

Second: The duration of 9,192,631,770 periods of radiation emitted by a specific electronic transition in the cesium-133 atom.

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Ampere: The constant current which if maintained in two straight parallel conductors of infinite length and 1 meter apart in vacuum, would produce a force between these conductors of 2 x 10 -7 newtons per meter of conductor length. If one applies 10 volts across a 10resistor, 1 ampere of current will flow through the circuit. is the capital greek symbol usually denoting ohms, the standard measure of electrical resistance. Voltage E, Current I, and Resistance R are related by:

E = IR

Kelvin: The kelvin is the unit of thermodynamic temperature and is equal to 1/276.13 of the temperature of the triple point of water (temperature at which water can exist as a solid, liquid, or vapor depending upon the pressure). The melting point of ice is 273K, room temperature is 298K, and water boils at 373K. To convert from degrees Centigrade to Kelvin, add 273.15. Example: 100 °C + 273.15= 373.15K (the boiling point of water expressed in kelvin).

Mole: A mole of material contains 6.023 x 10 23 particles. A mole of carbon atoms weighs 12.011g (the atomic weight of carbon). One can think of a mole as a number of objects. Just as one can have 5 pencils, one can have a mole (6.023 x 10 23 ) of pencils.

Dimensional Analysis: Regardless of units nearly all physical measures in the universe have dimensions

M

ab

L T

c

where M is mass, L is length, and T is time, and a, b, and c are integers. It is evident from Table 1.2 that for voltage, a=1, b=2, and c=-3. Equations can be checked for validity by ensuring these three numbers are the same on both sides of the equal sign. This is called dimensional analysis and is a useful tool

The System International set of unites, abbreviated SI, has conveniently defined the internation unit of Mass to be the Kilogram, the international unit of Length to be the Meter, and the international unit of Time to be the Second.

Table 1.2 Names and Symbols for Derived SI units

 Physical quantity Name of SI unit Symbol Definition of unit force newton N m kg s -2 pressure, stress pascal Pa m -1 kg s -2 (=N m -2 ) energy joule J m 2 kg s -2 power watt W m 2 kg s -3 (=J s -1 ) electric potential volt V m 2 kg s -3 (=J A -1 ) electric resistance ohm Ω m 2 kg s 3 A -2 (=V A -1 ) frequency hertz Hz s -1

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Force: That which changes the state of rest (or motion) of matter. The rate of change of momentum is a measure of force.

Force = mass x acceleration

In SI units, one newton is the force that will accelerate a one kilogram mass one meter

per second, per second.

Pressure (force per unit area). Popular units include pounds per square inch and (PSI), Torr, Bar,, atmospheres, and Pascals (Newtons per square meter). Pressure is a force distributed over an area. Absolute pressure is measured with respect to zero pressure (denoted PSIA), and gauge pressure is measured with respect to atmospheric pressure (denoted PSIG). If your car tire has about 30 PSIG, then it has about 45 PSIA (atmospheric pressure is about 15 PSI).

Energy: The capacity for doing work. Potential energy is stored energy due to the relative position of a body. Kinetic energy is the energy of a moving body;

Potential energy = mass x gravity x height.

Kinetic energy = 1/2 x mass x (velocity) 2

Power: The rate at which work is done. Power in watts will be obtained if work in joules

is divided by time in seconds.

Power = work / time

Electrical Potential: The work expended moving a charged body from point A to point

B in an electric field.

Electrical Resistance: For a conductor of electricity, resistance is the relationship of applied electric potential to voltage. Ohm's Law states that:

electric potential = current x resistance

Frequency: The rate of oscillation of a particle, wave or body. SI units are cycles per second (cps) commonly also called Hertz (Hz).

All of the metric (and some English) units use prefixes to make the expression of very large or very small numbers more clear. The kilo prefix in kilometer is probably the most familiar unit prefix. Below, in Table 1.3, the prefixes used in conjunction with metric units are listed along with their symbols and values.

Table 1.3 Names and Symbols for Derived SI units

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 Multiplication Factor Exponent Prefix Symbol 1,000,000,000,000,000,000 10 18 exa E 1,000,000,000,000,000 10 15 peta P 1,000,000,000,000 10 12 tera T 1,000,000,000 10 9 giga G 1,000,000 10 6 mega M 1,000 10 3 kilo K 100 10 2 hecto h 10 10 1 deca da 0.1 10 -1 deci d 0.01 10 -2 centi c 0.001 10 -3 milli m 0.000001 10-6 micro µ 0.000000001 10 -9 nano n 0.00000000001 10 -12 pico p 0.000000000000001 10 -15 femto f 0.0000000000000000001 10- 18 atto a

By this point you're probably saturated with technical jargon, so let's work together on an application of the material covered so far.

Example:

The mean radius of the earth is approximately 6,378,245km. Let's express the figure using SI units and prefixes. that figure using SI units and prefixes:

6,380 ,000 km = 6.38 × 10 6 km = 6.38 × 10 9 m

Sample Problems:

1.7 Fill in the table below using SI units

12,900 m

km

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 0.0023 g mg 0.067 A mA 12,300,000 N MN 0.000054 Pa mPa 1786 W kW 456 V kV 67,000,000 Ω MΩ 0.0000054 g µg 2 x 10 6 Pa MPa 345,000 Hz kHz 0.0034 V mV 3,400 g kg

1.8 If the meter is the SI unit for length, what would be the SI unit for area and volume?

1.9 Given that Ohm's Law states that Voltage = Current times resistance, what current would you expect in a circuit when a 10mV potential is applied across a 50Mresistor?

UNIT CONVERSIONS

Often it will be necessary to change from one system of units to another. A technique for performing unit conversions is given below and tables of conversion factors, grouped by function are given in Appendix B.

Let's work a simple example first, then examine the technique.

If you are driving at 30 miles per hour, how many feet per second are you traveling?

This problem requires that we change two sets of units; miles to feet and hours to seconds. Lets do the miles to feet conversion first. We know that there are 5,280 feet in

a mile, therefore we can write:

Now, let's change feet per hour to feet per second. Since there are 60 minutes in an hour and 60 seconds in a minute, we can calculate that there are 3600 seconds in an hour. This conversion factor (3600 sec/hour) will allow us to write:

 158,400 feet 1 hour 1 minute 44 feet × × = hour 60 minutes 60 seconds second

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Now, you notice that in the first conversion (miles to feet) we multiplied the conversion factor (5,280 feet/mile) by the original value of 30 MPH, but in the second step (converting feet per hour to feet per second) we divided. The trick here is to multiply always by 1, and organize the units to cancel algebraically.

Sample Problems:

1.10 Express the values in the left column in terms of the units in the right column.

 0.5 atm Torr 375 cubic feet liters 7.65 inches cm 0.004 psi Torr 450 cubic feet per minute liters/second

BASIC PROPERTIES of MATTER

For the purposes of our study of vacuum technology, matter may be divided into three physical categories or states: solid, liquid and gas.

Solids: The most ordered state of matter. Atoms and molecules of solids tend to remain in fixed positions with respect to one another. Solids have a definite shape and volume. Solid material may be crystalline or amorphous. Examples of crystalline solids include natural crystals, such as gemstones, and metals. Metals are typically composed of many micro-crystallites (grains) that usually require a powerful microscope to observe. Glasses have solid-like behavior (they have definite shape and volume), but on an atomic scale, there is no long-range atomic or molecular order, as exists in crystals. Glasses have been described as "super cooled" liquids.

Liquids: The state of matter in which atoms and molecules are relatively free to move about with respect to one another. Liquids have a definite volume, but the shape of a liquid is defined by the walls of its container.

Gas: The state of matter in which atoms or molecules move about freely with respect to one another, and tend to distribute themselves to fill any container, regardless of size.

About 400 BC, Greek philosophers argued that indivisible units of matter, called "atoms" existed, and they were the building blocks from which everything was made. Current understanding of the nature of matter includes a portion of this classical atomic theory. The indivisible building blocks that our physical world is made up of are called Elements. Familiar materials such as iron, carbon, oxygen and mercury are examples of elements. Compounds, on the other hand are materials that are formed from elements through a chemical reaction. Table salt, water and methane gas are all compounds. One very interesting feature of compounds is that they are composed of elements in definite ratios. For example, water molecules are always composed of two atoms of hydrogen and one atom of oxygen. Usually the physical properties of compounds are radically

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different than those of their constituent elements. Water, for example, is a liquid at room temperature, and yet both of its elements, oxygen and hydrogen are gases at room temperature. Not all material we are exposed to is in the form of compounds. Mixtures are simply physical combinations of materials (no chemical reaction involved). The air that we breathe is a mixture of approximately 79% nitrogen (a gaseous element at room temperature and atmospheric pressure) and 19% oxygen (another gas under the same conditions).

INTRODUCTION to MEASUREMENT TECHNIQUES

There is little point in setting up an experiment, and observing some physical (or chemical) phenomena unless one is prepared to record and later report meaningful information (data). In this section we hope to provide guidelines for use in this endeavor. First of all, one must think through the entire experiment before it is started to ensure that the procedure to be followed will result in a meaningful observation. Let me give you an example. I was working on a project, the goal of which was to use the characteristic emission lines of iron to determine when a sputter-etching process had gone to completion. I was using an existing vacuum chamber with a pyrex window view port for my spectrometer. Several days of data collection and analysis provided inconclusive results, so I began to wonder what I was doing wrong. As it turned out, the pyrex window was strongly absorbing the light I was hoping to observe in the vacuum chamber. After replacing the pyrex window with one made of sapphire, the results were in good agreement with what I had expected. Before beginning an experiment, you should at least have a guess (scientists call these theories) as to what will happen. In many of the vacuum pump experiments you will perform you will be measuring the pumping speed as a function of pressure. How do you expect the pump speed to change with pressure? Will the rate of change be constant? These are the kind of questions you would do well to consider before the experimental measurement. Another aspect of good data collection technique is to repeat the measurement enough times so that you are confident in the results.

Statistics: The science of the meaningful interpretation of data. Let's assume you're performing a set of experiments to determine the length of time required to pump a vacuum vessel from atmospheric pressure to 50 microns. You make four runs and the values recorded are: 124, 136, 118 and 144 seconds respectively.

Average: The sum divided by the number of measurements.

Average = (124+136+118+144)/4 = 522/4 = 130.5, which rounded to the correct number of significant digits is 131 seconds.

Range = 144 - 118 = 26 seconds.

For this very limited data set one could say that the time required to achieve a pressure of 50 microns is the average value plus or minus half the range. An acceptable way to present this data would be:

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Average time to achieve a pressure of 50 microns starting at atmospheric pressure in a series of four measurements was observed to be 131 seconds ± 13 seconds.

Notice that the measurement conditions (beginning and ending pressure), number of measurements (four), and the units (seconds) are all clearly stated.

Sample Problem:

1.11 Find the average and range for the following set of pressure

measurements: 1.2 x 10 -5 Torr, 1.8 x 10 -5 Torr, 2.1 x 10 -5 Torr, 3.1 x 10 -5 Torr and 2.6 x 10 -5 Torr.

PRESENTATION of DATA

Clarity of data presentation is very important. Your work, both in this laboratory course, and in your vocation, will be judged not only on its correctness, but on the manner in which it is presented. Prior to collection of a set of measurements, set up a table to enter your data in as the experiment progresses. Columns should be provided for the variables such as time, pressure, temperature, etc. It is good practice to record along with your table of data the time and date, your name, what experiment is being performed.

Table 1. Pump down data for diffusion pump experiment. Data recorded by Tom Jones on 6/21/90 at 6:30PM

 Elapsed time(sec) Foreline press (mTorr) Chamber Press (Torr) 0 30 6.0 x 10 -4 30 26 2.0 x 10 -4 60 22 8.0 x 10 -5 90 20 5.0 x 10 -5 120 18 8.0 x 10 -6

Graphs: Pictorial representation of data that allows one to view the relationships between variables. In this laboratory you will be constructing graphs of time versus pressure and pumping speed versus pressure. Typically, the horizontal (X) axis is used to plot the independent variable (such as time), and the vertical (Y) axis is used to plot the dependent variable (whose value depends on or is a function of the independent variable). We have created below a data table using the integers from 1 to 50 as the independent variable (X) and have calculated the dependent variable values (Y) for several simple functions.

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 X Y=1/X Y=X^2 Y=X^3 Y=Log(X) Y=Exp(X) 0 0 0 1.00E+00 1 1.0000 1 1 0.000 2.72E+00 2 0.5000 4 8 0.301 7.39E+00 3 0.3333 9 27 0.477 2.01E+01 4 0.2500 16 64 0.602 5.46E+01 5 0.2000 25 125 0.699 1.48E+02 6 0.1667 36 216 0.778 4.03E+02 7 0.1429 49 343 0.845 1.10E+03 8 0.1250 64 512 0.903 2.98E+03 9 0.1111 81 729 0.954 8.10E+03 10 0.1000 100 1000 1.000 2.20E+04 11 0.0909 121 1331 1.041 5.99E+04 12 0.0833 144 1728 1.079 1.63E+05 13 0.0769 169 2197 1.114 4.42E+05 14 0.0714 196 2744 1.146 1.20E+06 15 0.0667 225 3375 1.176 3.27E+06 16 0.0625 256 4096 1.204 8.89E+06 17 0.0588 289 4913 1.230 2.42E+07 18 0.0556 324 5832 1.255 6.57E+07 19 0.0526 361 6859 1.279 1.78E+08 20 0.0500 400 8000 1.301 4.85E+08 21 0.0476 441 9261 1.322 1.32E+09 22 0.0455 484 10648 1.342 3.58E+09 23 0.0435 529 12167 1.362 9.74E+09 24 0.0417 576 13824 1.380 2.65E+10 25 0.0400 625 15625 1.398 7.20E+10 26 0.0385 676 17576 1.415 1.96E+11 27 0.0370 729 19683 1.431 5.32E+11 28 0.0357 784 21952 1.447 1.45E+12 29 0.0345 841 24389 1.462 3.93E+12 30 0.0333 900 27000 1.477 1.07E+13 31 0.0323 961 29791 1.491 2.90E+13 32 0.0313 1024 32768 1.505 7.90E+13 33 0.0303 1089 35937 1.519 2.15E+14 34 0.0294 1156 39304 1.531 5.83E+14 35 0.0286 1225 42875 1.544 1.59E+15

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Y

50

40

30

20

10

0

Y = X

0
10
20
30
40
50

X

Figure 1.1 The plot of Y=X

Y = X^2

2500
2000
1500
1000
500
0
0
10
20
30
40
50
Y=X^2

X

Figure1.2 The plot of Y=X 2

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Y = X^3

120000
100000
80000
60000
40000
20000
0
0
10
20
30
40
50
Y = X^3

X

Figure 1.3 The plot of Y=X 3 .

Y = Log(X)

2
1
0
0
10
20
30
40
50
Y = Log(X)

X

Figure 1.4 The plot of Y=Log(X).

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Y = Exp(X)

7
10
6
10
5
10
4
10
3
10
2
10
1
10
0
10
0
5
10
15
Exp(X)

X

Figure 1.5 The plot of Y=Exp(X)

As with tables of data, clarity in presentation of graphical data is very important. Each graph should have labeled and scaled axes. The label should include the appropriate units.

In the example graph below, the independent variable (time) is plotted on the horizontal (X) axis, while the two dependent variables (chamber pressure and foreline pressure) are plotted on the left and right vertical axes, respectively.

Edwards E0-2 Diffusion Pump /Alcatel 2004 rotary Vane Backing Pump

.1
20
Tom Jones
Data recorded 6/21/90
Table 1
18
Convectron gage measurement at
pressures above 1 mTorr
16
.01
14
Ion Gage measurement below 1 mTorr
12
.001
10
8
6
.0001
Chamber press. [Torr]
4
Foreline Press [mTorr]
2
0
0
0
5
10
15
20
25
30
Chamber press. [Torr]
Foreline Press [mTorr]

Time [min]

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Mathematics-

Technical Mathematics with Calculus, 2 nd ed., Calter, Paul, Prentice Hall, Unglued Cliffs,

NJ, 1990.

Statistics-

Understanding Statistics, Mendenhall, and Ott, L., Duxbury Press, Div of Wadsworth

Publishing, Belmont, CA, 1972.

Elementary Statistics, 3 rd ed., Johnson, R.R., Duxbury Press, Div. of Wadsworth Publishing, Belmont, CA, 1980.

Physical Properties of Matter- CRC Handbook of Chemistry and Physics, Weast, R.C.,ed., CRC Press, Inc., Boca Raton, FL, 70 th edition, 1990.

SI Units- ASTM Metric Practice Guide, (ASTM E 380-76), American Society for Testing Materials, 1916 Race St., Philadelphia, PA, 1976.

Answers to Chapter 1 Sample Problems

 1.1 2 5 = 32, 10 3 = 1000, 56 0 = 1 1.2 4 0.5 = 2, 10 -4 = 0.0001, 625 1/4 = 5 1.3 23, 1200, 660, 1.3 x 10 -5 1.4 Log(2 5 x 3 2 ÷ 4 3 ) = 5 x Log(2) + 2 x Log(3) - 3 x Log(4) = 0.65 1.5 Log(4 3 ) = 3 x Log(4) = 1.81 1.6 Log (56 x 12) = Log(56) + Log(12) = 2.8 1.7
 12,900 m 12.9 km 0.0023 g 2.3 mg 0.067 A 67 mA 12,300,000 N 12.3 MN 0.000054 Pa 54 mPa 1786 W 1.786 kW 456 V 0.456 kV 67,000,000 Ω 67 MΩ 0.0000054 g 5.4 µg 2 x 10 6 Pa 2 MPa 345,000 Hz 345 kHz

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Vacuum Technology 60A & 60B

 0.0034 V 3.4 mV 3,900 g 3.9 kg

1.8 m 2 (square meters), m 3 (cubic meters).

1.9 10 -3 V = current x 5 x 10 7 , current = 20 nA.

1.10 Express the values in the left column in terms of the units in the right column.

 0.5 atm 380 Torr 375 cubic feet 10,620 liters 7.65 inches 19.43 cm 0.004 psi 0.21 Torr 450 cubic feet per minute 210 liters/second

1.11 Average value = 2.2 x 10 -5 , range of data = 1.9 x 10 -5 .

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Vacuum Technology 60A & 60B

Chapter 2: Safety

Our concern for the safety of everyone participating in this laboratory course is paramount. To achieve this goal, the Vacuum Technology Laboratory has been equipped with such safety features as smoke detectors, automatic sprinklers, fire extinguishers, and a first aid kit. Exposure to liquid chemicals has been minimized by the use of OSHA approved containers and exhaust gases are removed through a special ventilation system. Please use these physical safety measures that have been provided as they were intended; if you do not understand their function or proper use, please ask an instructor. The information presented in this chapter is only a summary of the material we felt was most important to provide for student safety awareness. In the final assessment, each individual is responsible for the safety of everyone in the laboratory.

Physical Safety

Eyes: Approved laboratory safety glasses (available at the bookstore) are required to be worn whenever any experimental work is being conducted in the laboratory. If you would like to use some of the laboratory time to perform calculations or plot data, we suggest moving to the campus library (it will be quieter there anyway).

Clothing: Many of the experiments involve the use of motor driven mechanical pumps.

It is strongly encouraged that no excessively loose fitting clothing (ie: neckties, scarves, very loose shirt sleeves) be worn while working on this equipment. Long hair that may be caught in the pulley of a mechanical pump is also a possible hazard; please tie back or otherwise prevent long hair from being entangled in any motorized device.

Skin Rupture: Sharp objects, including tools and vacuum system components may, if used or handled incorrectly result in tearing the skin. Beyond the physical discomfort of

such an occurrence, there exists a real danger of injection of chemicals and infection. If

a skin rupture occurs, immediately flush the area with clean water and apply pressure

using a clean cloth or towel, if bleeding is profuse, notify the instructor and if necessary, go to the school infirmary. An injured person should be accompanied to the infirmary either by another student or an instructor.

Sample Problem:

2.1 List three possible ways in which equipment (vacuum vessels, pressure vessels,

etc.) could fail causing projectiles to be scattered in the laboratory.

Electrical Safety

Electric shock is a major cause of fatalities at R&D and production facilities. Surprisingly, the most likely victim of an electrical accident is an experienced person with the equipment being used. Electricity is used to power some portion of every experiment that will be performed in this laboratory course. Generally, this electrical energy is well contained, so we are protected from its effects, and may become

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complacent with electrical safety measures. Almost everyone has experienced a mild electrical shock. The result is an unreasonable expectation that one will survive future electrical shocks. Electricity is uniquely dangerous because it is invisible. The danger that exists is that electrical hazards may surface in unexpected locations, and be undetected.

Electric Shock: Passage of electrical current through some part of the body. The current may be alternating (AC) or direct (DC) and vary from being so low in magnitude to be detected to so high as to cause fatality. Our bodies may incur damage by two mechanisms: damage to the nervous system and joule heating. Nervous System Damage: External mA range current input into the body causes pain by stimulating nerves in our skin. As applied current increases, control of muscles is lost and cramping occurs, often preventing an individual from releasing the source of current. Further damage may result if the electrical signals that control our involuntary muscles such as the heart, lungs and other vital organs is scrambled so as to prevent the proper operation of these organs. This may cause the heart to stop beating. Joule Heating: In a resistive heating element, current passing through live tissue will meet with resistance, causing heat to be generated. This heat can cause severe third degree burns along the path of the current, which may include vital organs.

Sample problem:

2.2 Electrical resistance through various parts of the human body is given in the table

below. Calculate the current flowing in each case, and after reading the next section on physiological effects, enter the effect for each part of the body.

 Body Part Voltage Resistance Current Physical effect ear to ear 110 V 100Ω head to foot 110 V 500Ω dry skin 110 V 600 kΩ

Physiological effects of electrical current passing through the body.

 SAFE DEFINITIONS 1 mA no physical sensation 1 to 8 mA sensation of shock-no muscle spasms (5 mA max safe current) UNSAFE DEFINITIONS 8 to 15 mA Painful shock. Muscle control is not lost. 20 to 50 mA Painful shock. Local muscle control is lost. 100 to 200mA Normal Heart beat affected. Victim holds onto current source as long as current flows. Death may result. > 200 mA Severe burns. Muscular contraction is so severe that chest muscles clamp the heart and stop it for the duration of the shock. If current continues, for several minutes, the heart may be too weak to restart after the flow of electricity is stopped.

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What to do in the case of a severe electrical shock:

1)

Call for help immediately.

Call loudly to other people in the immediate area. Have a person telephone for emergency medical services, specifying the incident and location.

2)

Rescue the victim.

Locate and safely de-energize the source of electrical power. Take extreme caution not to expose yourself to the electrical hazard. If necessary, use an insulated implement (dry broom handle) to remove the victim from the current source.

3)

Apply CPR.

Apply CPR as soon as possible if the victim is not breathing.

4)

Continue to give aid.

Continue CPR Until a medical rescue team arrives. Electrical shock victims have been revived from up to an hour after the electrical shock occurred.

5)

Get the victim medical attention.

Even if the victim appears to have recovered, a professional medical examination is required to check for invisible internal injuries.

Basics of Electricity

Electrical energy: The flow of electrons in a conductor.

Potential: The ability of an electric field to do work; the ability to cause motion of a charge. Electrical potential is expressed in volts (V).

Current: The flow of electrons; expressed in amperes (A).

Resistance: The degree to which a material allows the flow of electrons; units: ohms ().

Power: The time rate of energy transport or transformation; watts (W).

Frequency: Number of periods of a wave form per unit time; hertz (Hz).

DC: Direct Current. A constant (with time) electrical potential; may be positive or negative.

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DC

0
Voltage

Time

AC: Alternating current. The voltage of an ac current source varies sinusoidally with time. House current is 60 cycle (60Hz) AC.

Alternating Current

Voltage

Time

RF: radio frequency alternating current; typically kilohertz to gigahertz frequency.

The different current wave forms have different effects on the human body. For

example; AC causes heart fibrillation and muscle spasms. DC causes muscle clamping, heart seizures and burns at a higher current level than AC. RF alternating current passes through the skin readily and causes burns at much lower voltages than AC or

DC.

Capacitors: Electrical devices that store electrical energy. Many of the power supplies and control units used with vacuum equipment have capacitors in their circuits. Severe injury can result from coming into contact with a charged capacitor.

Always assume that a capacitor is fully charged

Before beginning any work with a circuit that has a capacitor, de-energize the capacitor using a grounding strap designed for that purpose.

Hazards Related With Electrical Equipment

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Vacuum Technology 60A & 60B

Fire: Many fires are initiated by electrical causes. Be familiar with appropriate electrical fire extinguishing techniques. Fire extinguishers have information on their labels regarding their proper use, read the label before the emergency.

Toxic gas evolution: Electrical energy may cause the chemical breakdown of insulating materials and the decomposition of gases (creating ozone for example). In addition, older capacitors may contain toxic PCB's.

X-rays: High voltage applied under vacuum will almost always result in the generation of X-rays. Appropriate shielding is necessary to reduce radiation exposure to an acceptable level.

Bright light: Sparks and arcs can cause severe eye damage.

Radiation: Microwave and RF radiation from electronic devices can be a health hazard, especially over a long periods of exposure.

General Safety Criteria for Design and Construction of Electrically Powered Laboratory Equipment:

 1) Buy good equipment (UL listed); use equipment suited for the application for service). (rated 2) Provide physical barriers to prevent personnel from contacting energized conductors; enclose equipment operating above 50 volts. 3) Enclose and install interlocks to prevent serious electrical hazards from access while energized. 4) Identify hazardous areas with warning signs and flashing lights. 5) Design systems to fail in a safe mode. 6) Design equipment to allow adequate access for maintenance; allow for emergency exits; maintain access to labeled breaker boxes. 7) Provide sufficient lighting and ventilation. 8) Prevent exposure of personnel or electrical components to water and provide proper drainage to prevent water accumulation. 9) Provide adequate grounding to all metal enclosures, equipment, cabinets, and structural components; use low impedance (resistance) conductors rated for the maximum possible current. 10) Provide safety ground hooks in the vicinity of all high voltage equipment that is accessed frequently.

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Vacuum Technology 60A & 60B

 11) Install emergency shut-down switches in the location of system operation. 12) For energy storage devices, provide convenient discharge points for contact with a ground hook. 13) Provide power disconnection's for all electrical equipment; label disconnects. 14) Have electrical designs reviewed, document designs and reviews.

Characteristics of Electrical Equipment Used in Vacuum Technology

Sample Problem:

2.3 Use any resources available (manuals, equipment tags, etc. to complete the

following table.

 Equipment Name AC/DC Max. current Max. voltage Max. power Mechanical pump Diffusion pump Sputter-ion pump Resistance evap. power sup. Sputter power supply Ion gage controller

Chemical Safety

Some of the materials (solids, liquids, and gases) you may encounter are chemical health hazards. Examples are chlorinated and fluorinated solvents, and mercury. Care must be taken to store, use and dispose of chemicals in a safe and environmentally sound manner. Specific details for the proper handling of chemicals must be researched using materials safety data sheets (MSDS). All chemical producers are required by federal law to supply an MSDS for their products upon request.

Organic solvents: In this laboratory organic solvents are stored in OSHA approved fire safe red metal cabinets. Transfer the minimum amount of the appropriate solvent to a suitable container (ie: glass beaker) for use near the experiment. Do not expose flammable solvents to sparks, hot surfaces or open flames. Use these solvents only in a well ventilated area. Prevent exposure or contact of solvents to the skin. After use, return the unused (clean) solvent to the red metal storage can. Allow any rags saturated with solvent to dry thoroughly then dispose of in a fire safe container.

Mercury: The use of mercury in vacuum technology has greatly diminished, but one should still be aware of the hazards involved with the use of this element. Mercury has an appreciable equilibrium vapor pressure under laboratory room conditions (2x10 -3 Torr). The toxic effects of mercury are cumulative, and cause irreversible damage to the brain and kidneys. Mercury should be stored in a tightly sealed non- breakable

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Vacuum Technology 60A & 60B

container (polypropylene) and handled so as to minimize contact with skin, ingestion and inhalation of its odorless vapor.

Mechanical Safety

Pneumatic Lines: Compressed air often provides a robust and compact energy source for the actuation of vacuum valves and other pneumatic devices. This is often provided at a pressure between 70 and 120 PSIG. Always wear safety glasses when working around live pneumatic lines, as plastic tubes carrying this pressure can whip through the air wildly if they become disconnected. Never attempt to cover the end of a line with your finger tip, as air can be directly injected through the skin into the body with painful or even fatal results.

Vacuum Gate valves: These often generate high actuation forces and one should never reach through a gate valve without first disconnecting the pneumatics. Gate valves are often actuated with a small electropneumatic pilot valve (frequently referred to as a solenoid) that frequently require continuous power to remain open. A PG&E power failure at eactly the wrong moment could crush bone or even cause dismemberment.

Thermal Safety

Some of the equipment involved in vacuum technology operates at extremely high or extremely low temperatures and requires some attention to safety.

Equipment operating at high temperature: Diffusion pumps and evaporation processes. Second and third degree burns may occur if skin comes into contact with this equipment.

Equipment operating at moderately high temperature: Mechanical pumps, power supplies and electronic components.

Equipment operating at low temperature: Cold traps(LN2), cryosorption pumps, cryogenic pumps, liquid helium lines, and helium compressors.

Las Positas College

Vacuum Technology 60A & 60B

2.1 A flawed, fractured or misused glass vacuum vessel could implode; a vessel

could be over pressurized, causing it to explode; volatile gases in a vessel could ignite, causing an explosion; parts of a rotating mechanical device could fail.

2.2 Electrical resistance through various parts of the human body is given in the table

below. Calculate the current flowing in each case, and after reading the next section on physiological effects, enter the effect for each part of the body.

 Body Part Voltage Resistance Current Physical Effect ear to ear 110 V 100Ω 1.1 A death head to foot 110 V 500Ω 220 mA severe burns dry skin 110 V 600 kΩ 18 mA painful shock

2.3 Use any resources available (manuals, equipment tags, etc. to complete the

following table.

 Equipment Name AC/DC Max. current Max. voltage Max. power Mechanical pump AC 4 A 110 V 440 W Diffusion pump AC 16A 110 V 1760 W Sputter-ion pump DC 5 mA 4 kV 20 W Resistance evap. power sup. DC 15A 40 V 600 W Sputter power supply DC 1.5A 1 kV 1500 W Ion gage controller DC 0.1A 1.5 kV 150 W

Las Positas College

Vacuum Technology 60A & 60B

Chapter 3: Review of Basic Vacuum Calculations

Before we go any further, some time should be spent on some of the vocabulary specific to vacuum technology.

Vacuum: from a practical sense, vacuum may be defined as the condition of a gas under less than atmospheric pressure. Table 3.1: Vacuum ranges

 Vacuum Description Range Low vacuum 25 to 760 Torr Medium vacuum 10 -3 to 25 Torr High vacuum 10 -6 to 10 -3 Torr Very high vacuum 10 -9 to 10 -6 Torr Ultrahigh vacuum 10 -12 to 10 -9 Torr Extreme Ultrahigh vacuum below 10 -12 Torr

Vacuum technology is based upon the creation of an environment in which a process (thin film deposition, electron beam welding, etc.) can be carried out. This normally implies that one remove air from a system to some acceptable sub atmospheric pressure by the use of some type of vacuum pumping equipment.

Atmosphere: The blanket of gases that surrounds the surface of the earth and extends outward to a distance of about 25 miles is referred to as "air" or "the atmosphere". This mixture of gases exerts a pressure that presses uniformly on all objects on the surface of the earth. This pressure is about 15 pounds per square inch at sea level.

Table 3.2: Composition of Dry Air

 Gas Partial Pressure [Torr] Percent [by volume] nitrogen 593 78.1 oxygen 159 20.9 argon 7.1 0.934 carbon dioxide 0.25 0.033 neon 1.4 x 10 -2 0.0018 helium 4.0 x 10 -3 0.00053 methane 1.5 x 10 -3 0.0002 krypton 8.6 x 10 -4 0.00013 hydrogen 3.8 x 10 -4 0.00005 nitrous oxide 3.8 x 10 -4 0.00005 xenon 6.6 x 10 -5 0.0000087

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Vacuum Technology 60A & 60B

Properties of Systems Under Vacuum

If we remove some amount of atmospheric gas from a leak-free vessel we will have created an environment that is drastically different in many respects: mechanically, chemically and physically.

Mechanical Effects of Vacuum: Have you ever placed a half full 2 liter plastic soft drink container that is at room temperature into a refrigerator, and noticed later after it has cooled that its sides are distorted and pulled inwards? What you have inadvertently done is create a condition in which the internal pressure of the plastic container was reduced, causing its surface to buckle. Vacuum engineers are acutely aware of this phenomenon, and design vacuum vessels to be sturdy enough to withstand the external atmospheric pressure of 14.7 pounds per square inch (at sea level) in the absence of compensating internal pressure. Structures and components that are particularly susceptible to distortion under vacuum conditions include flat, unsupported surfaces, thin sections, and flexible lines or bellows.

Sample Problem:

3.1 Calculate the approximate total force that will be exerted on a 4" diameter glass

view port used in a vessel under high vacuum

conditions.

Chemical Effects of Vacuum: The removal of gases from a container will reduce the number of gas atoms that are available to interact with materials in the container. For this reason many materials that are hydroscopic (have a tendency to absorb water from the atmosphere) are stored under vacuum. Materials that readily oxidize are also often stored either under high vacuum, or in an inert atmosphere (nitrogen or argon gas) after the air has been removed from the storage vessel.

Sample Problem:

3.2 List as many reactive elements or compounds that you know of which you would consider storing under vacuum or inert gas conditions.

Physical Effects of Vacuum: Many of the physical properties of gases are strongly

affected by the pressure of the gas. Thermal conductivity, electrical conductivity, propagation of sound, optical transmission, optical absorption are just a few. In addition to the effect of reduced pressure on the physical properties of gases, under vacuum solids and liquids also show markedly different behavior. Liquids, such as water, can be made to boil in a vacuum vessel without the application of heat. This occurs as soon as

the vapor pressure of the water exceeds that of the vacuum environment

atoms of solid material under vacuum conditions will spontaneously leave the surface of

the solid. The rate at which materials vaporize under vacuum is a function of the pressure in the system and the vapor pressure of the material. A more in-depth discussion of vapor pressure will be presented later.

Similarly,

Sample Problem:

3.3 We have suggested that physical changes in the thermal and

conduction of gases are brought about by a decrease in pressure. What are the trends

electrical

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Vacuum Technology 60A & 60B

you would expect in these two physical characteristics as pressure is decreased from atmospheric? (Increase or decrease?)

Gas Laws

Gases are composed of independent, randomly moving atoms or molecules that spontaneously expand to fill any container. The collective behavior of these atoms or molecules in a contained volume can be described when one knows any three of the four following quantities:

1. Pressure:

2. Volume:

3. Temperature:

4. Amount:

The force per unit area a gas exerts on its surroundings. (in our calculations we will use primarily Torr or atmospheres).

The internal capacity of a container, or vessel. (Liters)

The temperature of a gas is a function of its kinetic energy, that is, how vigorously the gas atoms are vibrating. Temperature must be specified in terms of an absolute temperature scale. We will use the kelvin scale (K=°C + 273).

The number of gas atoms in a volume (can be in terms of atoms or moles). {A mole of material is 6.02 x 10 23 particles}.

Boyle's Law: Under conditions of constant temperature, Boyle's Law gives the relationship between volume and pressure for a fixed quantity of gas.

P 1 × V 1 = P 2 × V 2

Let's do a thought experiment to demonstrate Boyle's Law. Imagine a system of two leak-free vessels as shown below.

TC1