Observations on Some Suggestions about Annealing

There are writings from a teacher attempting to make glass fusing simple.  Unfortunately, glass physics and chemistry are very complicated.  Attempting to avoid these complications leads to failures and other difficulties as the practitioner progresses. 

Proper annealing is one of the fundamentals to achieving sound kilnforming results.  Some suggestions have been made by a widely followed person to “simplify” the understanding of the annealing process.  Discussion of the meaning and importance of annealing can be found in many places, including here.  

Annealing temperatures

It has been suggested that the annealing temperatures can be inferred from the CoE of the glass that is being used. Discussion of what CoE is and is not can be found here and here.

Annealing temperatures are not directly related to the expansion coefficient (CoE) of the glass.  This can be shown from the published annealing temperatures for different glasses organised by presumed CoE:

·        “CoE96”: Wisssmach 96 - anneal at 482°C;  Oceanside - anneal at 515°C

·        “COE94”: Artista - anneal at 535°C

·        “CoE 93”: Kokomo - anneal between 507°C and 477°C – average 492°C

·        “CoE 90”: Bullseye - anneal at 482°C; Wissmach90 - anneal at 482°C; Uroboros FX90 - anneal at 525°C

·        “CoE 83”:

o   Pilkington (UK) float - anneal at 540°C;

o   typical USA float - anneal at 548°C;

o   Typical Australian float - anneal between 505°C and 525°C, average 515°C

This shows there is no direct relationship between CoE and annealing temperature.  Do not be tempted to use a CoE number to indicate an annealing temperature.  Go to the manufacturer’s web site to get the correct information.

Temperature equalisation soak

Annealing for any glass can occur over a range of temperatures.  The annealing point is the temperature at which the glass can most quickly be annealed.  However, the glass cannot be annealed if it is not all at the same temperature throughout the substance of the glass.  It has been shown through research done at the Bullseye Glass Company that a temperature difference of more than 5°C will leave stress within the glass piece. To ensure good annealing, adequate time must be given to the temperature equalisation process (annealing). 

From the Bullseye research the following times are required for an adequate anneal soak:

6mm /   1/4"            60 minutes

[9mm /  3/8"           90 minutes]

12mm  / 1/2"          120 minutes

[15mm  /   5/8"       150 minutes]

19mm   / 3/4"         180 minutes

[ ] = interpolated from the Bullseye chart for annealing thick slabs

Anneal Cooling

There are suggestions that a “second anneal” can be used on important pieces.  Other than observing that all pieces are important to the maker, the suggestion should be investigated.  On looking into the idea, it is essentially a second soak at 425°C, which is slightly below the strain point, rather than controlled cool from the anneal soak temperature.

It is reported that the Corning Museum of Glass considers 450°C as the lower strain point – the temperature below which no further relief of strain is possible.  This means that any secondary soak must occur above 450°C rather than the suggested 425°C. Such a soak is unnecessary if the appropriate cooling rates are used. 

Cooling Rate

Except in special circumstances, the cooling rate needs to be controlled as part of the annealing process.  Soaking the glass at the anneal is not the completion of the annealing.  Most practitioners follow the practice of choosing a slow rate of cooling from the annealing soak to some point below the strain point rather than a rapid one with a soak at the strain point temperature.

Annealing is not just the soak time (which is there to equalise the temperature), it is about the rate of the annealing cool too. The rate at which you cool is dependent on the thickness of the glass piece and whether it is all of one thickness or of variable thicknesses.

Even thickness

                                         Cooling rate

Dimension      time (mins)     1^st 55°C   2^nd 55°C

6mm              60                 83°C       150°C

9mm              90                 69°C       125°C

12mm            120                55°C       99°C

15mm            150                37°C       63°C

19mm            180                25°C       27°C

The “first 55°C” and the “second 55°C” refer to the temperature range below the chosen annealing temperature.  So, if you choose to anneal at 515°C, the “first 55°C” is from 515°C to 460°C and the “second 55°C is from 460°C to 405°C.  If you choose 482°C as the annealing temperature, the “first 55°C” is from 482°C to 427°C and the “second 55°C from 427°C to 372°C.

Tack fused/ uneven thickness

If your piece is tack fused, you need to treat the annealing rate and soak as though it were twice the actual total thickness. This gives the following times and rates:

Tack fused

Dimension (mm)                                Cooling rate

Actual     Calculated       time (mins)     1^st 55°C   2^nd 55°C

6            12                 120                55°C       99°C

9            18                 150                37°C       63°C

12          25                 180                25°C       27°C

15          30                 300                37°C       63°C

18          38                 360                7°C         12°C

Contour fusing required firing as though the piece were 1.5 times thicker.  Sharp tack or laminating requires 2.5 times the the actual thickness.

Fusing on the floor of the kiln

There is a further possible complication if you are doing your fusing on the kiln floor, or a shelf resting on the floor of the kiln.  In this case you need to use the times and rates for glass that is at least 3mm thicker than the piece actually is. 

Thus, a flat 6mm piece on a shelf on the floor would use the times and rates for 9mm: anneal soak for 90 minutes, anneal cool at 69°C to 427°C and then at 124°C to 371°C.  It would be safest if you continued to control the cooling to room temperature at no more than 400°C per hour.

But if it were a tack fused piece of a total of 6mm you would use the times and rates for 18mm.  This is using the rates for twice the total thickness plus the additional 3mm for being on the base of the kiln.  This gives the times and rates as being an anneal soak of 360 minutes and cooling rates of 7°C to 427°C and 12°C to 370, followed by 40°C per hour to room temperature.  Any quicker rates should be tested for residual stress before use.

Source for the annealing and cooling of fused glass

These times and rates are based on the table derived from Bullseye research, which is published and available on the Bullseye site.   It is applicable to all fusing glass with adjustments for differing annealing soak temperatures.

Annealing over multiple firings

It has been recommended by this widely followed person that the annealing soak should be extended each time subsequent to the first firing.  I am uncertain about the reasoning behind this suggestion. But the reasons for discounting it are related to adequate annealing and what is done between firings.

If the annealing is adequate for the first firing, it will be adequate for subsequent firings unless you have made significant alterations to the piece.  If you have added another layer to a full fused piece, for example and are using a tack fuse, you will need to anneal for longer, because the style and thickness have been altered.  Not because it is a second firing.  If you are slumping a fired piece, the annealing does not need to be any different than the original firing.

The only time the annealing needs to be altered is when you have significantly changed the thickness of the piece, or the style of fusing (mainly tacking additional items to the full fused piece).  This is when you need to look at the schedules you are planning to use to ensure your heat up is slow enough, that your annealing soak is long enough, and the cool slow enough for the altered conditions.

Determining the annealing point of unknown glass

You don’t have to guess at the annealing temperature for an unknown glass.  You can test for it.  It is known as the slump point test.

This test gives the softening point of the glass and from that the annealing point can be calculated.  This test removes the guess work from choosing a temperature at which to perform the anneal soak. The anneal temperature is important to the result of the firing.  This alone makes this test to give certainty about the annealing temperature worthwhile.

You can anneal soak at the calculated temperature, or at 30°C below it to reduce the anneal cool time.  This is because the annealing can occur over a range of temperatures.  The annealing occurs slowly at the top and bottom of the range. But is at least risk of "fixing in" the stress of an uneven distribution of temperature during the cool when the annealing is done at the lower end of the range.

Do not be fooled into thinking that CoE determines annealing temperatures.  Use published tables, especially the Bullseye table Annealing for Thick Slabs to determine soak times and cooling rates.  Use the standard test for determining the softening and annealing points of unknown glasses.

Further information is available in the ebook Low Temperature Kiln Forming.

Achieving the Striking Colour

"Is there anything special I have to do to fire striker glass?  Can I mix striker and non-striker in the same kiln or piece?"

Strikers generally need a two-hour soak at slumping temperatures, about 660C.  This heat soak helps ensure full development of the colour. If the soak is not long enough, the colour may not achieve the target colour at all, or be paler than anticipated.

The rate of advance to the heat soak is not critical.  But it does need to be the appropriate rate for the thickness and nature of the assembly of glass being fired.

If you were to have too short a heat soak, you can fire again to help mature underdeveloped colours.  This will, of course, change the profile of the finished piece.

Strikers are compatible within their manufacturer’s own range. So, they can be combined in the same piece as any other of the glass in the fusing compatible range.  That means that they can be fired in the same kiln load as non strikers.

The two-hour soak at slumping temperature will not harm the later stages of firing, but it might lead to use of a slightly lower temperature tack fusing than without the long heat soak.  That is because of the heat work put into the glass at the lower temperature.   Only observation will tell you how much less temperature is required.  It may be possible that only a little less time at the forming temperature is required.  Again, only observation will tell you that.

Strikers require a heat soak to mature the final colour.  These striking glasses are compatible with the rest of the fusing range from a single manufacturer. Glass from different manufacturers must be tested for compatibility before combined into a project.

Soaks Below the Softening Point

There are frequent suggestions that holds in the rise of temperature for glass are required.  Various justifications are given.  A few notes before getting to the explanation of why they are uncessary.

A note is required about the softening point sometimes called the upper strain point. There is a reasonable amount of discussion about the lower strain point.  So much that it is often simply referred to as the strain point.    Below the lower strain point, the glass becomes so stiff and brittle that no further annealing can occur.  Thermal shock can happen though, so the cooling needs to be controlled.

There also is an upper point at which the behaviour of the glass is different.  Above this temperature, no annealing can occur either, because the glass has become plastic and the molecules randomly arranged.  It is only just pliable, of course, but its molecules are no longer strongly bound to one another.  This is the temperature at which much of slumping is done.

It is disputed whether such a point exists.  Still, in practical terms it is where the glass becomes so plastic that it cannot be temperature shocked.  The temperature of this “point” is approximately 45°C above the annealing point, rather than the temperature equalisation soak. 

Note that the temperature at which Bullseye recommends that the annealing soak should occur is a temperature equalisation point, which is about 33°C below the glass transition temperature - the point at which glass can be most quickly annealed.  The average glass transition point for Bullseye is 516°C.  Most other fusing glasses use the glass transition (Tg) point as the annealing temperature for the soak.  They or you could employ the Bullseye technique on thicker slabs of the glass by setting the temperature equalisation point 33°C below the annealing point, and soaking for the same kinds of time used in the Bullseye chart for annealing thick slabs.  In fact, this is what Wissmach has recently done with its W90 and W96 fusing glass ranges.  They now recommend 482C (900F) as the anneal soak temperature.

Now to the point of the post.

The soaks that are often put into schedules on the rise in temperature are justified as allowing the glass to equalise in temperature.  Glass in its brittle phase is an excellent insulator.  This means that heat does not travel quickly through the glass.  Consequently glass behaves best with steady and even rises in temperature (and correspondingly on the reduction in temperature).  Rapid rates risk breaking the glass on the temperature rise, no matter how many or how long the holds are.  

This means a slower rate of advance will accomplish the heating of the glass in the same amount of time, and in a safer manner, than rapid rises with short soaks/dwells/holds.  The slower rate of temperature increase allows the glass to absorb and distribute the heat more evenly.  This slow heating is most obviously required in tack fusing where there are different thicknesses of glass.  

This means that it is possible for thin areas of glass to heat up much more quickly than glass covered by different thicknesses of glass.  It also applies to strongly contrasting colours such as black and white, because they absorb the heat differently - black more quickly than white.

There are, of course, circumstances where soaks at intervals are required – usually because of mould characteristics, in slumping, and in pate de verre.

Sometimes people add a soak at the annealing temperature on the way up in their schedules.  This is unnecessary.  If the glass has survived up to this point without breaking, it is highly unlikely it will break with a further increase in the rate of advance unless it is very fast.  The temperature after all, is above the strain point meaning the glass is no longer in the brittle phase.

Many people add a soak at around 540°C (ca. 1000°F) into their schedule on the increase in temperature, before their rapid rate of advance to the top temperature.  The choice of this temperature relates to the lower strain point.  This also is unnecessary, except possibly for very thick pieces. By this time the glass has reached its plastic stage and if it hasn’t broken by then, it won’t with a rapid rise in temperature either.

Further information is available in the ebook Low Temperature Kiln Forming.

Soaks at various temperatures during the advance to the upper strain points of glass are not necessary.  What is necessary is a knowledge of when the glass becomes plastic in its behaviour, and an understanding of how soaks can overcome characteristics of moulds, or how to achieve specific results and appearances of the glass.

Sintering

This is a process used in glass to stick glass together without any change in appearance of the separate pieces.  It has various names - fuse to stick and lamination are two.

General description
“Sintering or frittage is the process of compacting and forming a solid mass of material by heat or pressure without melting it…. Sintering happens naturally in mineral deposits [and] as a manufacturing process used with metals, ceramics, plastics, and other materials.

“The atoms in the materials diffuse across the boundaries of the particles, fusing the particles together and creating one solid piece. Because the sintering temperature does not have to reach the melting point of the material, sintering is often chosen as the shaping process for materials with extremely high melting points such as tungsten and molybdenum….
 
“An example of sintering can be observed when ice cubes in a glass of water adhere to each other, which is driven by the temperature difference between the water and the ice.”
https://en.wikipedia.org/wiki/Sintering
 
Applied to glass this means that you can make a solid piece out of multiple touching or overlapping pieces that do not change their shape.  This is done by using low temperatures and very long soaks. 
 
The usual process is to take the glass at a moderate rate up to the lower strain point.  The rate of advance is slowed to 50°C or less to a temperature between slumping and the bottom of the tack fuse range.  The operator must choose the temperature, largely by experimentation. 
 
The slow rate of advance allows a lot of heat work to be put into the glass.  This, combined with a long soak (hours), gives the molecules time to combine with their neighbours in other particles.
 
Sintering can be done in the range of 610°C to 700°C.  The lower limit is determined by the strain point of the glass being used and practicality.  

The upper limit is determined by the onset of devitrification. This  has been determined by the scientific studies of sintered glass as a structure for growing bone transplants.  Devitrification reduces the strength of the bonds of the particles at the molecular level.  These studies showed that the onset of devitrification is at 700°C and is visibly apparent at 750°C regardless of the glass used.  Therefore, the choice was to use 690°C as the top sintering temperature. 
 
For reasons of practicality the lowest temperature tested was 650°C.  Indications were that at least an additional two hours would need to be added to the sinter soak for each 10°C reduction below 650°C.  This would make for a 12-hour soak at 610°C.  For me this was not practical.
 
My recent testing has indicated some guidelines for the sintering process:
 
The ramp rate has significant effects on the strength of the resulting piece. 

• A moderate rate (150°C) all the way to the sintering temperature needs a two-hour soak at the top temperature. 
  
• A rapid rate (600°C) - as used in medicine – to the sintering temperature requires approximately six-hours soaking.
• A rapid rise to the strain point followed by the slow 50°C per hour rate to the sinter temperature requires a three-hour soak.

 
The temperature range of 610°C to 700°C can be used for sintering.  The effects of the temperature used have these effects:

• With the same rates and soak times, lower temperatures produce weaker glass.
• The lower the temperature, the longer the sinter soak needs to be for similar strengths.  Generally, the soak at 650°C needs to be twice that of sintering at 690°C.
• Lower temperatures produce more opaque glass.  In this picture all the glass is clear powder and fine frit in the ratio 1:2, powder:frit.

 

The annealing of sintered objects needs to be very cautious. The particles are largely independent of each other, only joined at the contact points.  The annealing soak needs to be longer and the cool slower than for simple tack fusing. 

• Testing showed that annealing as for 12mm is adequate. 
  
• There was no advantage of annealing as for 25mm as that did not increase the strength.

 
Porosity
Although the structure of the sintered glass appears granular, it is not porous except at or below 650°C.  At the lower temperatures, the glass becomes damp on the outside and weeps water.  At 670° and 690°C the outside became cool to touch but did not leak water.  This observation depends on evenly and firmly packed frits.
 

Grain structure at 650C

Grain structure at 690C

The keys to successful sintering of glass are the use of a heat work through slow ramp rates, and long soaks throughout the whole firing.

Further information is available in the ebook Low Temperature Kiln Forming.

Anneal soaks

An odd concept was presented recently.  This in summary was that if you have long soaks on the way up to top temperature you do not need to have such a long anneal soak as normal.

This is a fundamental misunderstanding of the physics of glass.  As the glass temperature rises above the upper strain point (about 55°C above the annealing point), the molecules become disordered.  No amount of soaking at any temperature on the way up to the top temperature will change that. 

The glass (and the molecules of it) will need to be cooled relatively quickly from the top temperature to avoid crystallisation of the glass.  This is the reason for the fast cool to the annealing soak.  It is also a reason to avoid a soak at approximately 50°C above the annealing point – there is a slight risk that crystallisation could form.  This would appear as scum marks on the surface, rather than in the interior.

Whatever soaks you have performed on the way to top temperature, you will need the full length of soak for the full or tack fuse.  And you will need it for the slump too.

No amount of soaking on the way up to top temperature in kilnforming will have any effect on the requirements for the annealing soak at the cooling part of the schedule.  The soaks in the early part of the schedule, no matter how many or how long, do not change the annealing requirements.

More detailed information is available in the e-book: Low Temperature Kilnforming.

Odd Schedules

Schedules appear on the internet which do not seem to have a logical sequence in the firing schedule.  Some have multiple soaks at intervals up to 540°C.  Others have kind of dance toward the top temperature – slow, quick, slow.  Some initially cool at a given rate and then slow to about half that initial rate.

Multiple soaks

These schedules have been referred to as catch-up schedules.  They tend to look something like this:

200°C to 150°C for 20 minutes

250°C to 300°C for 20 minutes

300°C to 590°C for 20 minutes

50°C   to 677°C for 30 minutes

330°C to 804°C for 10 minutes

AFAP   to 482°C for 60 minutes

60°C   to 370°C for  0 minutes

Off

The justification for the first two soaks is given as allowing the glass to catch up to the air temperature.  It would be much safer for the glass to have a moderate steady advance in temperature rather than risking the heat shocking of the glass.  You could achieve the same work in the same amount of time by altering the rate of advance to a single one of 198°C to 590°C.  This achieves the same temperature in the same amount of time, but has less risk of heat shock, as there is a steady input of heat.  

Secondly, if the glass can survive the initial rate of heat up without breaking, there is no need to soak at an arbitrary temperature.  The first relevant point where a change in temperature makes sense is above the softening point, which for most fusing glasses is about 540°C. The equivalent softening point for float glass is about 700°C

Slow, quick, slow

This kind of schedule alters rates up and down with little justification as far as I can see.  This is an example:

139°C  to 560°C  for 30 minutes

222°C  to 621°C  for 30 minutes

139°C  to 786°C  for 15 minutes

9999 to  515°C  for 120 minutes  

60°C   to 427°C  for 10 minutes

115°C  to 350°C  for 10  minutes

The question for me is why the slow down to top temperature. There is a lot of heat work being put into the glass, so that the higher top temperature may not be required.  The slower rate from 621°C does allow a form of a bubble squeeze to occur, but is not the traditional one.  A 139°C rate from 621°C to 677°C with a soak would be faster than usual, but may be acceptable.  I would prefer 50°C per hour with a 30-minute soak at the end.  Then advancing at 300°C per hour to top temperature.  The anneal soak and cool of this schedule are acceptable, even though different than I would do it.

Erratic Slumping Schedule

The fusing schedule above was followed by this slumping schedule:

83°C to 148°C  15 minutes

167°C to 590°C  10 minutes

83°C to 720°C  10 minutes

222°C to 410°C  120 minutes

83°C to 427°C  10 minutes

This schedule seems to have a catch-up phase in that it goes at half speed for the first 148°C and then doubles the speed to 590°C (a little above the brittle phase of the glass).  It then slows the rate and continues that to a very high slump temperature.  It is, of course, necessary to have a slower rate of advance in the slumping than the fusing, as the piece is now thicker. Slowing the rate of advance as much as in this should be able to achieve the slump at around 620°C (100°C) less than the target temperature used by the schedule. 

Once the top temperature soak is finished, a very slow cool to the annealing soak is used in this schedule.  This is not ideal as it invites devitrification to form.  The kiln and its contents should be allowed to cool as quickly as possible to the temperature equalisation soak at the annealing point.

The schedule then uses an annealing soak temperature 100°C below that used for the fusing. This does not make sense. The annealing soak should be at the same temperature for both firings.  The length of the soak is not in question, but the early turn off the kiln at 427°C is questionable. The anneal cool of the fused piece extended down to 350°C.  The anneal cool on slumping should be almost the same as the fuse.  Almost all anneal cools extend to 370°C at least.

Anneal Cools

Some anneal cools have erratic rather than progressive cooling.  In this example the early part of the schedule is eliminated:

……………..

AFAP to 482°C 120 minutes

110°C to 427°C 0 minutes

55°C to 370°C 0 minutes

200°C to 100°C 0 minutes

off

Here the schedule is faster in the most critical part of the anneal cool than in the next, cooler part.  This will not provide as good an anneal as if the first two segments after the equalisation soak were reversed.  Start slowly in the anneal cool and then you can speed up (approximately twice the previous segment rate) on each of the following segments.

Rationale

This critique of the schedules above is not to batter anyone.  It is to make clear that there needs to be a conscious rationale for each of the segments in relation to the others.  If you take a schedule from a source, it is a good idea to see if there is a reason for each segment and how it relates to the next. 

·        The scheduling must take account of the nature of the glass.  Glass is a poor conductor of heat and needs steady moderate input of heat.

·        Glass is brittle until approximately 55°C above the annealing temperature when you can accelerate the rate of advance.

·        Time is required to allow air out from between the layers of glass. This usually done in the range of 620°C to 675°C and is known as the bubble squeeze.

·        You need to go relatively quickly through the devitrification range of temperatures – approximately 700°C to 760°C - both up and down.

·        Glass needs a temperature equalisation soak at the annealing point (or nearby) related to its thickness.

·        The rate of cooling needs to be progressive.  The first 55°C below the annealing soak is the most important.

·        Cooling rates must be related to thickness.

·        The second cooling rate can be up to double the initial one.

·        The final cooling rate can be double the previous one.

·        The rate of firing will affect the required top temperature.

Pot Melt Temperature Effects

When firing a pot melt, you have to consider how high a temperature you wish to use.

Viscosity is reduced with higher temperatures so increasing the flow and reducing the length of soak, although there are often some undesirable opacifying effects.

The size of the hole is also relevant to the temp chosen. The smaller the hole, the higher the temperature will have to be to empty the pot in the same amount of time. Of course, you can just soak for longer at a lower temperature to achieve the desired object of emptying of the pot without changing the temperature.

Using the same principle, the larger the hole the lower the temperature required to empty the pot in a given amount of time.

The temperature used to empty the pot will need to be between 840C and 925C. The problem with temperatures in the 900C to 925C range is that the hot colours tend to change, e.g., red opal tends to turn dark and sometimes become brown. Some transparent glasses also opacify. There is also the possibility that some of the glasses will change their compatibility.

So the best results seem to come from temperatures in the 840 to 850C range with longer soaks than would be required at 925C - possibly 4 or more hours.

Also remember to give melts a longer than usual anneal as they will be thicker than 6mm at the centre - somtimes as much as twice the edge thickness.