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The Laboratory Companion a Practical Guide to Materials, Equipment, And Technique

The Laboratory Companion a Practical Guide to Materials, Equipment, And Technique

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Pure quartz glass, lead glass, borosilicate glass, or any other type of glass that is
clear is in phase. In-phase glass is completely homogeneous throughout. Glass
that has any cloudy nature to its appearance can easily be discerned as being out
of phase or has phase separation. The cloudy nature is due to inseparable phase
(or materials) from the glass phase. As mentioned, glass is glass because it cools
too fast for the molecules to align themselves into their crystalline structure. If
there are nucleating agents that can enhance the growth of crystals or if the glass
is held at too hot a temperature for too long, some crystallization will occur.
Sometimes phase separation can be visually desirable such as that which occurs
in opaline glass. By placing an earth alkali fluoride or phosphate material on the
surface of the glass, the quickly generated fine-crystalline surface disperses light
so efficiently that an opal glow is created. Photosensitive glass is an excellent
example of a more practical/commercial use of phase separation. This phase sepa-
ration is activated by ultraviolet light; and once the ultraviolet light is removed,
the glass rephases to the glassy state.
Phase separation is not always a surface phenomenon. The glass that is eventu-
ally changed into a pyroceramic material has a nucleating agent mixed throughout

6

Materials in the Lab

the original vitreous material. After the object has been formed and examined, it is
slowly baked through its phase separation in an oven.
Vycor®, a high-temperature glass that often can be substituted for quartz glass,
is also made by a phase separation process (see page 16).

The phase separation producing opalescence and photosensitivity are produc-
tion-created. That is, during the production of the glass, the phase separation
occurs. The phase separation that occurs with pyroceramic material and Vycor
requires baking the glass at high temperatures for an extended time. This elevated
temperature provides the time for the molecules to align and/or separate them-
selves in a crystalline pattern.

Unfortunately, not all phase separation is desirable. When borosilicate glass is
heated for too long near its annealing temperature, a phase separation will occur.
This tends to exhibit itself throughout the glass, but can only be observed with an
electron microscope. Despite it not being observable to the naked eye, the ramifi-
cations of this separation are considerable. The glass separates itself into two
phases: One is rich in silicic acid, while the other is rich in alkali borate.5

The
result of this change is that the glass has much greater sensitivity to chemical
attack.

The significance of the chemical attack sensitivity can best be demonstrated by
heat exchangers that must deal with high-temperature water. There are several
issues and conditions that come together for this effect:

1. Heat exchangers are made of thick glass.

Because thick glass requires a longer annealing process, there is a
greater opportunity for phase separation to occur.6

2. Due to the manufacturing process, they must go through the annealing

process several times.

Phase separation is a result of the total length of time the glass is
held to high temperatures, not the length of time at any one setting.

3. Glasses with high alkali content are more susceptible to chemical

attack.

Water is not generally thought of as a caustic material, but it can be
to less chemically resistant glass (e.g., lead and soda-lime glass). Even
soda-lime glass that has too great a percentage of soda is more chemi-
cally vulnerable than a soda-lime glass with a lower percentage of soda.
Generally, borosilicate glass is generally very resistant to water. How-
ever, if the alkali concentration is too high (due to phase separation) and
this glass is subjected to high-temperature water (more corrosive than
room temperature water), greater glass erosion can be expected.

Glass 1.1

7

Because the thick glass (of a heat exchanger) that had been annealed several
times is now confronting hot water,* it is more likely to fail (corrode and break)
than other borosilicate glassware.
Aside from being initiated by sitting in hot ovens for too long a period of time,
phase separation can also occur when a glass is worked too long or too often. This
is why glass can only be repaired a limited number of times. After too many
repairs, glass devitrifies (or recrystallizes, a symptom of phase separation) while
being worked (see next section), and this devitrification does not disappear by
heating. There are five items to consider for limiting the possibility, or degree of
phase separation due to annealing operations1

^
1. All annealing procedures to which an article is subjected before comple-
tion must be added together.

2. The number of annealing steps should be kept as small as possible

3. Since the level of the annealing temperature and the duration of the
annealing method tend in the same direction (i.e., phase separation),
these should be limited whenever possible.

4. The annealing temperature should not exceed 550°C.

5. Each separate annealing period should not exceed 30 minutes. Should an
article have to be annealed several times, the sum of all annealing
periods should not exceed two hours.

Regardless of the heating processes, phase separation will occur if the glass was
not cleaned prior to annealing. Salts (from finger prints), silicone grease, water
spots, and other contamination can "burn into" the glass, creating nucleation
points from which phase separation will originate.

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