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NATL INST OF STANDARDS & TECH R.I.C.

NBS

PUBLICATIONS

All 10261 6433

Smith, L. E/Predictlon ot the long term QC100 .U56 NO.86-3474 1986 C.2 NBS-PUB-C 3474

Prediction of the Long Term

Stability of Polyester-Based

Recording Media

L. E. Smith

D. W. Brown

R. E. Lowry

U.S DEPARTMENT CF COMMERCE

National Bureau of Standards

institute for Materials Science ana Engineering

Polymers Division

Gaithersburg, MD 2C899

Progress Report to June 1986

QC for 100 il Archives

.1155 gtcn, DC 20403

#86-3474

1986

c.2

NBSIR 86-3474

RESEARCH

INFORMATION CENTER

PREDICTION OF THE LONG TERM

STABILITY OF POLYESTER-BASED

RECORDING MEDIA

L. E. Smith

D. W. Brown

R. E. Lowry

U.S. DEPARTMENT OF COMMERCE

National Bureau of Standards

Institute for Materials Science and Engineering

Polymers Division

Gaithersburg, MD 20899

Progress Report to June 1986

Prepared for National Archives

Washington, DC 20408

U.S. DEPARTMENT OF COMMERCE, Malcolm Baldrige, Secretary

NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Director

Prediction of the Long Term Stability of PolyesterBased Recording Media

by

Leslie E. Smith, Daniel W. Brown, and Robert E. Lowry

National Bureau of Standards

Gaithersburg, MD 20899

Abstract

Magnetic data tapes have been aged at several temperatures and relative

humidities. Data previously recorded on the tapes was read back after aging

and the inability to read such data was used to make a preliminary estimate of

tape lifetime. Based on this criterion we estimate a useful tape lifetime of

20 years at ambient conditions. This involves a long extrapolation, however,

because there have been few failures at humidities lower than 100% and

temperatures below 85° C, and only one failure at all below 60° C. The tape

lifetime estimate should be considerably more certain by the time of the final

report in this series which will be issued in November 1987. There are

documented reports of tape failure after ten years of storage under normal room

temperature and humidity and we have seen cases of failure after only a few

years so the lifetimes can vary considerably.

Reading failures with rapidly-aged tapes appear to be caused primarily by

exudation of material from the binder layer. This accumulates on the reading

heads or makes the tape stick to the tape transport. In order to test the

condition of tapes before failure, three tests were devised that measure

adhesion or extensibility of the binder layer. Water content and weight

changes on aging were also measured. None of these five measures correlated
quantitatively with the ability of a tape transport to read data previously

written on the tapes, but some of them are useful indicators of risk.

1.0 Introduction

Information storage on microfilm and magnetic tape offers higher storage

density and more rapid access than corresponding paper records. They

constitute a large fraction of current data and have become important parts of

many libraries and archives. The expected useful lifetime of these materials

at ambient conditions is long but not known. Since October 1980, the National

Archives and Records Administration has sponsored research at the National

Bureau of Standards aimed at defining the effects of storage environment,

developing tests of the condition of the materials, and predicting the lifetime

of film and tape. This is the fourth progress report on this research, others

being NBSIR 82-2530, 83-2750, and 84-2988 [1,2,3]. Magnetic tapes have been

the subject of almost all the work in this reporting period.

Photographic film and magnetic tape consist of different active coatings

on a film of poly (ethylene terephthalate) (PET). The stability of PET film was

previously investigated in this program and it was concluded that it should

retain useful properties for over 500 years at 20° C and 50% relative

humidity(RH) [2].

The ferromagnetic material of the magnetic tapes in this study, small

particles of gamma ferric oxide, is suspended in crosslinked polyester

polyurethane which also serves to bind the magnetic particles to the supporting

film. Other materials such as lubricants, adhesives, or stabilizers are

frequentlyn added to this layer and in at least one formulation a second

coating without ferromagnetic particles is applied to the other side of the

2
supporting film. Polyester polyurethane is subject to auto catalytic

hydrolysis [4] , which was expected to limit the lifetime of the tape. Some

types of magnetic tapes contain chromium oxide particles which do affect the

chemical degradation mechanisms. This has recently been reported by

researchers at IBM [10]

.

Hydrolysis of the binder breaks fragments off the crosslinked network

which can be extracted by organic solvents. Cuddihy[5] extracted material from

aged tapes and concluded that tape aged at 100% and 30% RH contained increased

soluble material, as expected, but tapes aged at 11% and 0% RH contained less

soluble material than unaged tapes. We qualitatively confirmed these

observations on several brands of tape [2]. Indeed, most tapes appeared to

contain slightly less soluble material after aging even at relative humidities

as high as 30%.

Cuddihy[5] attributed this behavior to an esterification reaction between

acid and alcohol groups in the binder, essentially the reverse of hydrolysis.

However, we had found that uncrosslinked polyester polyurethanes slowly

hydrolyzed at 25% RH [43 . Thus there is an apparent inconsistency between the

results with magnetic tape and simpler polyester polyurethanes. Model binders

of crosslinked polyester polyurethanes without oxide particles were prepared

and aged. They also degraded with aging at 25% RH. We have also seen color

changes and increased nitrogen contents in binders aged at low humidities [3]

.

Neither of these observations is consistent with simple esterification so we

conclude that more complex crosslinking reactions are taking place that

counteract the effects of continuing hydrolysis. Such reactions would also

explain the differences in behavior between tape binders and uncrosslinked

model polymers.

3
Tape lifetime can be limited by detachment of binder from the supporting

film. The binder may become weaker due to degradation and fail cohesively or

the bond between the binder layer and the support may decrease and cause

adhesive failure. Either would be revealed by measuring the force required to

peel binder from the support. A preliminary test procedure was developed and

measurements made that revealed large decreases in peel force due to aging

under some conditions [3]

Digital data were written on and read from aged and unaged tapes using a

tape transport under computer control. Problems were encountered in reading

some aged tapes after several reading cycles [3].

Our approach to estimating tape lifetime is to write data on tapes, age

them at known temperatures and relative humidities, read the data on the tape

after aging, and alternate agings and reading attempts until the tape becomes

unreadable. Lifetimes will then be known which can be extrapolated to estimate

a value under typical storage conditions. Note that the total number of times

a tape has been read increases linearly with the number of aging periods.

An easy way of monitoring tape condition during storage is highly

desireable because of anticipated uncertainty in the estimate of tape lifetime.

Other tests were developed with this consideration in mind. The quantities

measured were: (1) the force required to peel the binder from the support; (2)

the elongation of the tape at which the binder separates from the support; ( 3 )

the number of rolling translations of a crease required to separate the binder

from the support; (4) the water content of the tape at 45% relative humidity;

and (5) the change in weight of the tape during aging. It will be seen that

these five quantities change during aging. The peel force, rolls to detach

4
binder, and elongation for binder separation vary greatly, but the changes do

not consistently correlate with tape lifetime.

2.0 Experimental Procedures

Data was encoded in 1/2 inch-wide tapes at a density of 1600 bpi using a

9-track tape drive of the tension-arm type. The drive is capable of speeds up

to 75 ips. A reflecting marker signaling logical BOT was placed about 5 meters

from the free end of the tape, the tape advanced to the load point, and a

standard label as required by the operating system was written on the tape.

The number 1023456789 was then written, initially 100,000 times, but later

48.000 times when the supply of original tape became depleted. We used the

system default setting of 2048 bytes for the block size. The number was made

negative every.10, 000 or 12,000 numbers. Another reflecting marker was

attached and the tape was rewound and read on the same drive. The negative

numbers were printed to show that reading had been successful. A section of

tape containing the numbers was cut from the reel about 5 meters beyond the

second reflecting marker. Pieces of tape were from 15 to 25 meters long,

depending on how many numbers had been written.

The pieces of tape were formed into loose coils, about three inches in

diameter, and weighed after equilibration in a room maintained at 45% relative

humidity and 22°C. They were then placed in jars containing small bottles of

water or aqueous salt solutions, chosen to give relative humidities of 100, 75,

50, or 25%. Salts used were potassium chloride, sodium chloride, sodium

dichromate, and calcium chloride giving relative humidities of 85, 75, 54, and

30%, respectively [6 , 7] . Aging took place in the jars in ovens thermostatted at

85, 60, and 35° C.

5
2.1 Reading Data from Aged Tapes

Aged tapes were equilibrated as above, weighed, and the differences

between initial and final weights were recorded. Tapes were then read 10 times

if possible. Several tapes aged at 85° C did not have a readable label block

after the first short aging period. These were rewritten, aged again, and

almost always successfully read. We suspect the initial problem was caused by

a dimensional change but have no proof of this. Such behavior was not counted

as tape failure because of the subsequent successful write and reads. The

final number and the time consumed in reading were printed out after each read.

Tapes that gave difficulty were tried a second time after cleaning the heads of

the tape transport.

Unreadable tapes showed one of several behavior patterns. Sometimes the

label block was unreadable, as above, but the tape could not be rewritten.

More frequently, tapes could be read one or more times with failure to read

occurring at a non-integral number of reads. The reading program printed the

approximate location of the difficulty in such failures. Another mode of

failure was for the tape to stick in the tape transport. Such tapes sometimes

developed a puckered edge because of the stress. Occasionally, tapes would

become sticky, and crease and wind on the driving capstan of the transport.

This pulled tape off the take-up reel as well as off the supply reel and

damaged the tape transport because the tension arms were suddenly released when

the tape came off the takeup reel.

A small amount of material was transferred from many aged tapes to the

tape transport, even from tapes that were read successfully. These deposits

were most conspicuous on the read and write heads but also were found at other

6
places along the tape path, particularly on the urethane rubber-coated capstan.

A swab soaked in ethanol was used to clean the read and write heads after each

piece of tape was tested and the whole tape path was cleaned after about ten

tapes had been tested.

Subsequent to the reading test, pieces were cut from an end of the tape

for measurement of peel force and rolls and elongation for separation. Tapes

that had been read successfully were reequilibrated as above, reweighed, and

aged for another period.

2.2 Peel Force Measurements

The adhesion of the binder layer to the PET support was measured by a

somewhat different method than described in the previous report. The current

test is similar to that used in ANSI X3. 40-1983 but modified to make it more

reproducible for the very small force measurements required with aged tape.

Results reported here were obtained by applying a 20 to 25 cm long piece of

1/2-wide tape, sticky on both sides, to an aluminum or plastic bar. One cm of

the sticky tape on what would become the upper end of the bar was masked so as

to provide a non-sticky surface. A somewhat longer piece of the tape to be

tested was applied to the bar, magnetic side to sticky tape, which was then

suspended from a load cell. A piece of sticky tape with an attached string was

then applied to the non-magnetic side of the top end of the tape to be tested.

The other end of the string went around a 1/4-inch diameter shaft mounted in a

high-torque, variable-speed, electrically-driven laboratory stirrer. This

stirrer was directly below the load cell. The string had some slack to permit

the stirrer to get up to speed quickly. Turning on the stirrer pulled the

magnetic tape from the bar, almost always with transfer of binder to the sticky

7
tape. The combined length of sticky tape and magnetic tape was frequently

pulled from the bar unless the uppermost portion of sticky tape was masked as

described. The output voltage of the load cell was recorded. A visual average

of this was used to calculate the peel force. The length of chart between

initial deflection and final decrease of the deflection was used to calculate

the draw rate, although we found peel force was not very dependent on draw rate

over a wide range.

The principal advantage of the current test is that it strips binder from

all tapes. The test described in the last report was done at much slower draw

rates, which resulted in several unaged tapes retaining their binder. The

modifications also hold the angle of the peel constant whereas the angle of

unsupported tapes will vary somewhat with the stiffness of the tapes.

2.3 Binder Separation by Elongation

Upon aging the binder layer becomes stiff rather than elastic. If the

tape is stretched, the PET elongates but the binder layer cannot follow so it

cracks and separates from the support. The elongation at which this occurs is

an indication of the brittleness of the binder.

The elongation for binder separation was measured by mounting the tape to

be tested in a tensile tester with an initial jaw separation of four inches and

then stretching the tape at a draw rate of one inch per minute while gently

touching the binder side of the lengthening tape. Generally, the binder became

rough at some fairly specific elongation and came off the tape. This

elongation we call the elongation for binder separation. Some unaged and

mildly aged tapes broke, usually at more than 100% elongation, before the

binder separated. Some severely aged tapes also broke before the binder

8
separated, usually at about 1% elongation, even though they were still

generally readable in this condition.

2.4 Rolls for Binder Separation

A very simple qualitative test for binder separation was done by creasing

the tape, across the long direction, so that the binder side was on the outside

of the crease. This crease was translated back and forth along the tape by

rolling it between thumb and forefinger. No unaged tape lost binder in many

such translations. Aged tapes often lost binder, sometimes when creased and

sometimes after several passes between the fingers. The number of passes was

arbitrarily limited to a maximum of ten. Thus a value less than ten indicates

degradation in this test.

2.5 Water Content

Water contents were measured at various humidities by placing 10 to 20

grams of loosely coiled tape in a low flask with a 71/15 standard taper joint.

The flask and its separated top were placed in a large desiccator above a

saturated salt solution or if the dry weight was desired calcium sulfate

dessicant. Two days later the desiccator was opened and the top put in the

flask, which was weighed promptly. Equilibrium was approached from both

directions, except at dryness. Water content was calculated as the difference

in the weights of the tape when dry and at other relative humidities.

2.6 Precision and Accuracy

Peel force, elongation for separation, and the number of rolls for

separation are approximate measurements and subjective to some degree. Values

9
reported are reproducible to about 25% when the same operator does the tests.

Some of the imprecision may be due to environmental factors in the test area,

since there were days when many results were higher than had been found after

the previous aging period. A second worker, trained by the first and then

working independently, obtained values for the elongation for separation that

differed by as much as two times from those obtained by the first worker.

The mass of tape samples were determined on an analytical balance to about

0.5 mg accuracy. However, tapes of mass 10 g sorb about 0.5 mg, 0.005%, of

water for each percent relative humidity. Thus humidity control really limits

the accuracy of the result. Day to day changes in the mass of samples measured

in the room nominally at 45% RH suggest the imprecision in the mass is about 2

mg or 0.02%. Many of the mass changes during aging were not much more than

this. Percentages based on samples equilibrated in desiccators and weighed in

closed flasks ought to be precise to about .01%. Both of these estimates

assume the tape is at equilibrium.

3.0 Results

3 . 1 Tape designations

Table 1 codes the tapes used in this study. The first column lists the

numbers used in the last report and the second lists new numbers used to

simplify the coding. More tape has been obtained as needed. Three of the

manufacturers had changed the name of the tape during the time of this work and

reported to be making it by an improved process. Their tapes with the original

names were no longer available. The reorder number then designates the code of

these new tapes. All tapes except 6, 51, and 52 were premium tapes from major

manufacturers. Tapes 6, 51, and 52 are tapes sold but not manufactured by

10
other suppliers which designated tape as their premium grade. Tapes 51 and 52

are called their standard grade, nominally the same tape, but with a large

difference in initial peel force [3]. Tape 72, which had not been obtained at

the time of the last report, was available only for a short while and only a

little work was done with it.

3.2 Organization of results

The six dependent variables for each tape tested makes analysis of the

results rather difficult. The most direct way is to plot each quantity

measured for each tape aged at each condition versus aging time. This has been

done and all of the plots are included in this report, most of the them in the

Appendix. Our principal concern in this report is tape lifetime as a function

of aging condition. The other measurements of physical condition, while very

useful as indicators of tape condition, did not quantitatively correlate with

results of the read test. Therefore, values of peel force, elongation for

binder separation, rolls for binder separation, water content, and weight gain

on aging will be discussed only briefly.

3.3 Reading tests

Some of our preliminary experiments were surveys in which six brands of

tape were in one jar during aging at 100, 50, or 25% relative humidity. These

experiments will be called survey experiments in this report. Failed tapes

were not aged additionally so the environment of the unfailed tapes changed

with time. Some of the results are in Fig. 1-4, plotted as successful reads

versus aging time. Ten successful reads are plotted as some value between S

and 10 to avoid superimposing data from different tapes. Included in Fig. 1,

11
which contains all our data from aging at 85° C and 100% relative humidity, are

results from two pieces of tape 6, aged in their own jar. Figures 1-3 show

that decreasing relative humidity greatly increases the time to failure at

85° C. Figures 1 and 4 show that a lower aging temperature at 100% relative

humidity increases the time to failure.

3.3.1 Description of Failures

The supporting film of tape 51 broke as the tape was being loaded on a

reel after 203 days aging at 85c and 50% RH. This demonstrates that binder

degradation is not the only limit to tape lifetime even though it is the most

common.

To date, the only other tape in the survey experiments that can not be

read ten times is tape 1 which was aged at 60°C and 50% relative humidity, for

329 days. Other tapes have been read through 410 days aging under these and

milder conditions.

Most data comes from experiments using pieces of tape from a single

supplier in separate containers. Results of the read test from some of these

are in Fig. 5-8. Prefixes to the tape identifying numbers in the figure

legends equal the number of pieces aged. Pieces with the same aging history

which were read ten times or were read the same number of times give

superimposed lines on these plots. Occasionally different pieces of tape have

very different times to failure, tape 41 at 85°C and 75% relative humidity for

example. Usually tapes fail in the same or adjacent aging periods, showing

that behavior is reasonably reproducible. Tapes 21 and 41 lasted longer at

85° C and 50% relative humidity when aged individually than when aged with other

brands, suggesting that volatiles from one tape may affect another tape. The

line for tape 72 in Fig. 7 shows that failed tape does not necessarily fail

12
absolutely. In this case a few reads were possible even at times equal to

twice that of the initial failure and similar behavior has been seen with other

brands of tape.

Tapes 41 and 42 aged at 85° C and 75% RH for 86 days, Fig 5, actually broke

in the tape transport. The other tapes that are were read 10 times after this

much aging were capable of much less elongation than originally. Thus

lifetimes of several tapes may be limited by the degradation of the support

film.

Four pieces of tape 1 were read without difficulty after 242 days aging at

60° C and 50% RH, suggesting that the failure of this tape in the survey

experiment under the same conditions was related to the presence of other

brands of tape or was not at the low end of the 225-329 day range.

Aging under milder conditions has resulted in only two failures. Both

involved tapes that were initially aged without data and then were first

written after about 500 days aging. Tape 41, written after 534 days at 60°

C

and 25% RH, could be read only twice. Another piece of tape 41, written after

537 days at 35° C and 100% RH, could not be read at all at 722 days. Tapes

preaged at 35° C and 25% RH have been read after 1100 days total aging.

The binder layer of most of the failed tapes was scratched, even when no

deposit was obvious on the reading head. Usually any deposit on the heads was

white, suggesting that it contained little or no iron oxide. Scratched areas

are not transparent, indicating that the binder layer has not been completely

removed. Many aged but unfailed tapes also have scratches.

Tape 1 has always failed by sticking to the tape transport, generally by

wrapping around the capstan. It is the only tape tested that has a coating on

both sides of the supporting film with the back side non-magnetic . The capstan

13
bears against the non-magnetic side of the tape, so tackiness of the back

coating is disastrous. Such tackiness was noticed when the tapes were loaded

onto reels before the reading test because adjacent layers of the tape did not

slide over one another. Other tapes have behaved somewhat similarly on a few

occasions but they only followed the capstan part way around and then peeled

off with an abrupt snap. Degradation products may have moved from the magnetic

side to the back side of the adjacent layer making such tapes marginally tacky.

3.3.2 Attempts to Rejuvenate Tape

One tape that failed after slight progress into the data block was

completely read ten times after it had been hand wound so all of the data area

had passed over the read and write heads, which were then cleaned. A

substantial deposit had accumulated on the read and write heads. Wiping

another failed tape with an alcohol soaked swab did not make it readable.

Presumably the swab should also have removed deposits from the tape.

About ten attempts were made to rejuvenate failed tapes by aging them at

85 and 60° C over a desiccant. Only one such tape became readable.

3.3.3 Lifetime Estimates

Tape lifetime, defined as the aging time associated with failure to be

readable for 10 passes, lies in the interval between the end of the aging

period at which a piece of tape was read ten times and the end of the

subsequent aging period after which it could not be read ten times. Figure 9-

18 show these intervals for aging at 85 and 60° C as horizontal bars, the ends

of which show the interval described above. Symbols showing the maximum times

at which ten reads have been made are used if failure has not yet occurred.

Replicates are shown by plotting additional lines and symbols displaced by 2

- 5 \

from the actual relative humidities. Examination of these figures shows that

14
failures have generally been at 85° C at several humidities or at 60° C and 100%

RH.

A simple way to approach lifetime estimation at ambient conditions is to

treat lifetime, (LT) , as the reciprocal of a rate and use an Arrhenius

equation. Thus LT** 1 = A exp(-E/RT) so LT = [exp (E/RT) ] /A. Here E, R, T, and A

are the activation energy, gas constant, absolute temperature, and

preexponential factor, respectively. Consequently, plots of log LT versus

1000/T were made. Fig. 19-23. Data are too few to do more than demonstrate

general trends so an average lifetime is plotted for each tape aged at any

condition at which any sample of that tape had failed. Each average is the

arithmetic mean of the sum of the times at the midpoint of the appropriate bars

in Fig. 9-18 and the maximum number of days unfailed samples had been aged at

the same condition. Storage conditions are assumed to be about 20° C, (1000/T)

= 3.41, at 50% RH.

Linear extrapolation of the plotted lines is valid if the Arrhenius

equation is applicable. Lifetimes at ambient conditions estimated by this

procedure are approximately 20 years. However, the single failure that has

occurred to date at 35°C, with tape 41, has occurred earlier than predicted by

this linear extrapolation. Obviously, more data are required before any firm

conclusion can be drawn.

3 . 4 Results with other measured quantities

Table 2 contains the values of peel force, elongation for binder

separation, rolls to detach binder, and water content at 45% relative humidity

found for unaged tapes. More than 10 rolls were required to detach the binder

but the value listed is ten for all tapes. The quantities above provide an

15
indication of changes in properties of the tape although they do not correlate

in a definite way with ability to read the tape.

3.4.1 Peel force

The unit used for peel force is the number of grams required to separate

half inch wide tape from the binder layer. In the previous report, we

normalized the data to the width of the tape and reported the results in units

of Newtons/m. However, some of the tapes peel in patches and we are now

skeptical of the validity of dividing by the width.

Peel force of unaged tape is plotted versus peel rate in Fig. 24. Values

of force generally decrease with peel rate but we have ignored this effect in

working with the aged tapes because of the approximate nature of the

measurements. Peel rates are about ten times greater than used for the data in

the previous report. All tapes lost binder but some required quite high peel

rates before separation occurred. The force recorded is higher, about 1000 g,

if the binder is retained on the magnetic tape. Aged tapes generally peeled

easily so a peel rate of about 5 cm/s was used unless the binder would not come

off.

Fig. Al- A28 of the appendix show how peel force varies with aging time.

Each plot shows all results for one tape aged at one temperature. Rapid and

very great decreases to an approximately constant value occur at high

temperature and all relative humidities. Tape 1 retains a higher peel force

than other tapes. Aging at 35°C causes a substantial decrease in peel force at

100% relative humidity but results in a smaller change at 25% relative

humidity. All tapes behave in a qualitatively similar manner but the

percentage change in peel force is less for tapes with low initial peel force.

16
The lowest peel force found was 1 g. This value is probably relatively

uncertain but indicates an enormous change from any initial peel force.

However, several such tapes were read ten times without any difficulty. Some

tapes with higher peel forces could not be read ten times. Thus, a low peel

force does not guarantee a failure to read a tape but it does indicate a tape

in poor condition and a high probability of failure.

3.4.2 Elongation for binder separation

Fig. A29 - A55 show how the elongation for binder separation is affected

by aging. Aging at high temperature causes large, rapid decreases in

elongation for binder separation, except for tape 1. Aging at 35°C results in

lower elongations at 100% relative humidity but not at 25% relative humidity.

Tapes can remain readable long after the elongation values have become low but

some tapes could not be read 10 times when the elongation for binder separation

was 40%.

3.4.3 Rolls to detach binder

Fig. A56 - A76 show how the number of rolls less than 10 required to

detach binder from the tapes is affected by aging. Aging decreased the number

of rolls to very low values in some cases. Tape 6 seems particularly labile

since it was the only tape aged at 35° C for which rolls decreased. Tapes 1,

21, and 22 are particularly resistant to binder detachment. Some tapes could

be read ten times even when the rolls required had decreased to zero (binder

had flaked off when the tape was creased) . In some cases tape 21 was

unreadable when binder did not come off in ten rolls.

3.4.4 Water content of tapes

Fig. A77 - A83 show water content as a function of relative humidity for

aged and unaged tapes. The plotted symbols that appear to be error bars are

17
percentages obtained when equilibrium was approached from high and low

humidity. Symbols are plotted at the midpoint between these values. Aged

tapes are more hygroscopic than unaged tapes in all cases. Differences in

water content in aged and unaged tapes range from somewhat less than 0.1% to

0.

2% at 50% RH. Larger differences occur at higher humidities. Usually

equilibration was slower with aged tapes and was particularly slow when excess

water was desorbing. This is reflected in the longer bars through the symbols,

1.

e. the tapes were further from equilibrium.

Moving samples from one desiccator to another is a slow process. A room

with 45% RH was therefore used as the equilibration chamber, since it had

mechanical air circulation which speeds up the equilibration. Water content

measured in the room for a variety of aged tapes is plotted versus aging time

in Fig. A84 - A90. Water content is usually increased by aging, the more so the

higher the relative humidity. A few tapes, usually those aged at low relative

humidity show the same or lower water content as the unaged tape.

3.4.5 Weight changes of tapes during aging

The increased water content of tapes aged under certain conditions

suggested the possibility of monitoring aging by simply weighing the tape at

constant relative humidity. The anticipated storage environment ought to be at

approximately constant humidity, at least during certain periods of the year.

A 2000-foot long tape on its reel has a mass of about 900 g, of which the tape

is 600 g. Differences in water content of 0.1% equal 0.6 g. Balances are

commercially available that can accommodate the reel of tape and weigh it to 1

mg.

However, there was evidence that materials left the tape. White deposits

accumulated on the inner wall of the jars used for aging tape. Water used for

18
aging tapes at 100% relative humidity left a deposit when it was evaporated to

dryness. Conceivably, water content might increase but tape mass might

decrease due to loss of other materials. Tape mass were measured in the

controlled humidity room before and after aging. Fig. A91 - A96 are plots of

cumulative weight change versus aging time. Occasionally we did not make a

weighing and show this by discontinuing the line and starting it again in the

next complete interval. Usually weight gains were found in samples aged at

high humidity and weight losses were found in samples aged at low humidity.

There are several instances of initial weight gain at 75% RH followed by weight

loss, e.g.. Fig. A92, A93, A94, A95, and A96. This might mean that a severe

degradation generates volatile fragments. It appears that weight changes will

not serve to monitor tape degradation unless results at 35° C show more regular

behavior.

3.5 Naturally aged tapes

Some measurements have been made on tapes more than 10 years old. Results

of these are in Table 3. Tapes 11 and 33 have the same manufacturers as tapes

1 and 31, respectively. However, tape 11 does not have a back coat. Binder

layer is actually flaking off the outer layers of tape [8], which was the

portion used for the tests. The tapes had been kept in a reasonably clean

laboratory environment with little exposure to organic or acid vapors. The

years listed are those written on the reel. Initial values of the measured

quantities for these tapes are not known but only the current values for tape 3

appear very low. Peel force and elongation for binder separation of tape 33

are significantly lower than initial values for tape 32, but peel force for

tape 33 is about equal to the initial value for tape 31.

19
Some unreadable tapes written as early as 1972 were obtained from the Jet

Propulsion Laboratory, with the proviso that they were not to be tested

destructively. All of these tapes required more than 10 rolls to detach the

binder from the support. No other tests have been made. A worker there

commented that many old tapes could be read only once so that a tape testing

program involving random sampling might eventually destroy a substantial

portion of a tape library without finding bad tapes.

An entire box of cassette data tape was obtained and opened after seven

years of storage at laboratory ambient conditions. All of these tapes bind

badly in the cassette drive and an oxide colored deposit accumulates on the

read and write heads. Under some circumstances tape lifetimes at ambient

conditions can be considerably shorter than the 20 years we have suggested from

our accelerated tests.

4.0 Discussion and Future Work

No attempt will be made to discuss the lifetime measurements because there

are too few failures at less than 100% RH to properly appraise the situation.

More data will be obtained before the project is terminated.

Many factors have been measured that characterize general tape condition

but they do not correlate well with tape lifetime. That leads us to speculate

as to what aspect of accelerated aging does bring about tape failure, if ve

define failure as inability of the tape transport to read the tape. Failure to

read a particular bit has been attributed to a deposit pushing the magnetic

particles too far from the reading head to be detected [8]. Our tape transport

writes in nine tracks across the tape, eight data bits and a parity bit.

Correction for one unread bit in a byte is made from the parity bit. Thus two

20
bits in a single byte must be undetected for the tape to be unreadable. It is

our tentative conclusion that artificial aging causes materials to exude from

the tape binder, giving rise to deposits that cause failure. These may operate

by the mechanism above or cause the tape to stick in the tape transport.

Observations suggesting this are: (1) Head deposits were most frequently

observed from the more labile tapes, 1, 6, and 31; (2) Head deposits are more

often white than oxide colored; (3) Tapes without backcoating left deposits on

the capstan, which does not contact the magnetic side of the tape; (4) Tape 1,

the only back-coated tape, has the most pronounced tendency to stick when aged

at high humidity; (5) Scrapes and striations on failed tapes do not go through

the binder layer; (6) Dry aging of failed tapes does not rejuvenate them.

Bertram et al.[9j made an observation consistent with this conclusion.

They aged a tape at 55° C and 100% RH until it had an immeasurably high bit

error rate. The tape was wiped with a commercial wiping tissue and the error

rate dropped to 2xl0-6

.

It is uncertain whether the exuded material is an additive or a

degradation product. The fact that humidity has a strong effect on lifetime

seems more consistent with a degradation product than an additive, i.e. there

would not be sufficient sorbed water to change the phase diagram or affect the

migration of additives.

Tape aging and reading tests will be continued during the next year

including measurements on videotape which is now aging. Binder detachment

tests will be discontinued for tapes which already have suffered great

reductions in these values. An effort will be made to identify the materials

that come out of the tapes by use of infrared spectrometry. These materials

include jar deposits, materials in the humectant, and head deposits. Samples

21
of poly (ethylene terephthalate) and model binders are still being aged. Acid

contents of both materials and solubility characteristics of the latter will be

determined.

References

1. D. W. Brown, R. E. Lowry, and L. E. Smith, Prediction of the Long Term

Stability of Polyester Recording Media, NBSIR 82-2530, June 1982.

2. Ibid., NBSIR 83-2750, August 1983.

3. Ibid., NBSIR 84-2988, December 1984.

4. D. W. Brown, R. E. Lowry, and L. E. Smith, Macromolecules 13: 248; 1980.

5. E.F. Cuddihy, IEEE Trans. Magn. 16: 558; 1980.

6. D. S. Carr and B. L. Harris, Ind. Eng. Chem. 41: 203; 1949.

7. C. D. Hodgewan, Handbook of Chemistry and Physics, Cleveland, OH, Chemical

Rubber Co.

8. S. B. Geller , NBS Spec. Publ. 500-101, June 1983.

9. N. Bertram, A. Eshal, J.C. Mallinson and M. Wildman, Recording Media

Archival Attributes (Magnetic), Ampex Corporation, November 1979, p.93.

10. R. Bradshaw, et al., IBM Journal of Research and Development 30(2): 203;

1986.

22
Table 1. Tape Numbering Scheme

0-1.0. New # Reorder #

i 1 1

2 21 22

3 31 32

4 41 42

5A 51 No Reorder

5B 52 No Reorder

6 6 6 None 72 No Reorder

Table 2. Initial Tape Characteristics

Tape # Peel Force, g Elong. for Sep., % Rolls for Sep. , # H2 O wt

1 130 74 10 0.31

6 190 88 10 0.30

21 160 >96 10 0.25

22 320 >109 10 —

31 70 >107 10 0.27

32 440 >135 10 —

41 440 98 10 0.33

42 460 135 10 —

51 400 >145 10 0.32

52 20 79 10 0.30

72 320 >118 10 0.31

A > symbol means the tape broke at the listed elongation before the binder

separated.

Table 3. Characteristics of Tapes Stored at Ambient Conditions

Tape # Year Peel Force, g Elong. for Sep. , % Rolls for Sep. , #

8 1974 3 11 1974 94

33 1975 70

33

72

85

0

10

10

23
LIST OF FIGURES

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

Figure

1. Successful Reads Versus Time at 35 C and 100% RH

2. Successful Reads Versus Time at 85 C and 50% RH.

3. Successful Reads Versus Time at 85 C and 25% RH.

4. Successful Reads Versus Time at 60 C and 100% RH

5. Successful Reads Versus Time at 85 C and 75% RH.

6. Successful Reads Versus Time at 85 C and 50% RH.

7. Successful Reads Versus Time at 60 C and 100% RH

8. Successful Reads Versus Time at 60 C and 75% RH.

9. Lifetime of Tape 1 at 85 and 60 C.

10. Lifetime of Tape 6 at 85 and 60 C.

11. Lifetime of Tape 21 at 85 and 60 C.

12. Lifetime of Tape 22 at 85 and 60 C.

13. Lifetime of Tape 31 at 85 and 60 C.

14. Lifetime of Tape 32 at 85 and 60 C.

15. Lifetime of Tape 41 at 85 and 60 C.

16. Lifetime of Tape 42 at 75% RH at 85 and 60 C.

17. Lifetime of Tape 51 at 85 and 60 C.

18. Lifetime of Tape 52 at 85 and 60 C.

19. Log Lifetime of Tapes 1 and 6 Versus 1000/T.

20. Log Lifetime of Tapes 21 and 22 Versus 1000/T.

21. Log Lifetime of Tapes 31 and 32 Versus 1000/T.

22. Log Lifetime of Tapes 41 and 42 Versus 1000/T.

23. Log Lifetime of Tape 51 and 52 Versus 1000/T.

24. Peel Force of Tape Binder Versus Peel Rate.

24
SUCCESSFUL

READS

VERSUS

TIME

AT

85C

AND

100%

RH

DAYS

AGED
SUCCESSFUL

READS

VERSUS

TIME

AT

85C

AND

50%

RH ], O, A, +, X, *

TAPES

1,

21,

31,

41,

51,

AND

52

IN

ONE

JAR

TAPE

51

BROKE

WHEN

LOADED

AFTER

203

DAYS

AGING o

C\2 O

COo

C\2 O

COo

DAYS

AGED
SUCCESSFUL

READS

VERSUS

TIME

AT

85C

AND

25%

RH

100

200

300

400

DAYS

AGED
SUCCESSFUL

READS

VERSUS

TIME

AT

60

C

AND

100%

RH

O CO CO Tt* C\2 o

(ox = ox qnv 8 N3aM.aa aaiioid samvA) savaa

160

240

320

DAYS

AGED
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READS

VERSUS

TIME

AT

85C

AND

75%

RH 4

TAPE

1;

0,2

TAPE

6;

0,2

TAPE

21; ©, 2

TAPE

22; A, 2

TAPE

31; 2

TAPE

32; +, 2

TAPE

41; *, 2

TAPE

42; X,

TAPE

51; *.

TAPE

52 o

DAYS

AGED
SUCCESSFUL

READS

VERSUS

TIME

AT

85C

AND

50%

RH 3

TAPE

1;

<0,3

TAPE

6;

0,3

TAPE

21; ©, 1

TAPE

22; A, 3

TAPE

31;

100

150

200

DAYS

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TIME

AT

60

C

AND

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CO

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120

100

240

DAYS

AGED
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AT

60C

AND

75%

RH

<>, 2

TAPE

6;

0,2

TAPE

21; ©, 2

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160

240

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120

240

360

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LIFETIME,

DAYS
LIFETIME

OF

TAPE

6

AT

85

AND

60

C

85C,

FULL

LINES;

60C,

DASHED

LINES;

% ‘AJjamnH 3allvi3h

120

240

360

480

LIFETIME,

DAYS
LIFETIME

OF

TAPE

21

AT

85

AND

60

C

85C,

FULL

LINES;

60C,

DASHED

LINES;

85C,

A

,

60C,

LONGEST

TIME

TO

DATE

FOR

10

READS

AT

PLOTTED

CONDITION.

% ‘AuamnH SAiiviaH

120

240

360

480

LIFETIME,

DAYS
LIFETIME

OF

TAPE

22

AT

85

AND

60

C

85C,

FULL

LINES;

60C,

DASHED

LINES;

85C,

A

,

60C,

LONGEST

TIME

TO

DATE

FOR

10

READS

AT

PLOTTED

CONDITION.

% ‘AJjamnH 3allyi3h

120

240

360

480

LIFETIME,

DAYS
LIFETIME

OF

TAPE

31

AT

85

AND

60

C

85C,

FULL

LINES;

60C,

DASHED

LINES;

60C,

LONGEST

TIME

TO

DATE

FOR

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PLOTTED

CONDITION.

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120

240

360

480

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DAYS
55o

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120

240

360

480

LIFETIME,

DAYS
LIFETIME

OF

TAPE

41

AT

85

AND

60

C

85C,

FULL

LINES;

60C,

DASHED

LINES;

85C,

A

60C,

LONGEST

TIME

TO

DATE

FOR

10

READS

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PLOTTED

CONDITION. —

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120

240

360

480

LIFETIME,

DAYS
LIFETIME

OF

TAPE

42

AT

75%

RH

AT

85

AND

60

C

85C,

FULL

LINE;

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60C,

LONGEST

TIME

TO

DATE

FOR

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CONDITION.

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240

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120

240

360

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LIFETIME,

DAYS
LIFETIME

OF

TAPE

52

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85

AND

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C

85C,

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120

240

360

480

LIFETIME,

DAYS
1000/T

LOG

LIFETIME

OF

TAPES 1

AND 6

VERSUS

1000/T ,A

TAPE 1

AT

100,

75.

AND

50%

RH; +,X

TAPE 6

AT

100

AND

75%

RH.
1000/T

LOG LIFETIME, DAYS

O

LOG

LIFETIME

OF

TAPES

21

AND

22

VERSUS

1000/T

,A

TAPE

21

100,

75,

AND

50

%

RH;

X

TAPE

22

75%

RH.
LOG LIFETIME, DAYS

O

O

co

X o

o

4^

O

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LOG

LIFETIME

OF

TAPES

31

AND

32

VERSUS

1000/T

,O

TAPE

31

100,

75,

50

AND

25%

RH;

X

TAPE

32

AT

75%

RH
1000/T

LOG LIFETIME, DAYS

LOG

LIFETIME

OF

TAPES

41

AND

42

VERSUS

1000/T

A

,O

TAPE

41

100,

75,

50,

AND

25%

RH; X

TAPE

42

75%

RH.
1000/T

LOG LIFETIME, DAYS

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LIFETIME

OF

TAPE

51

AND

52

VERSUS

1000/T

A

TAPE

51

AT

100

AND

50%

RH;

+

,X

TAPE

52

AT

100

AND

75%

RH.
PEEL

RATE,

cm/s

LOAD,

g

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