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.

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.

Firing multiple layers

Glass Stela
Credit: Stephen Richard

Fusing multiple layers is prone to the creation of multiple large bubbles.  It also needs a strategy to schedule for thick layers.

Avoid bubbles

A widely recommended strategy for stacks of glass is to fire in pairs of layers. Then combine the fused two-layer pieces in a final firing. 

It is easier to fire two layers of glass than 6, 8 or 10 layers. The heat up is easier and less time consuming for multiples of 6mm than multiples of 3mm. The bubble squeeze schedule is simpler.  It also allows inclusions between the initial two-layer sheets and then between the layers of 6mm sheets.

This multiple firing strategy reduces the risk of large bubbles in a stack of multiple pieces. It seems the weight of the 6mm layers forces the air out from between the thicker glass more effectively than thinner layers. 

It is also a simpler set of firings.  If you were to want to make up a 12mm thick piece from 3mm sheets, your heat up will be very long compared to firing two layers in three firings.

E.g. Stone* recommends a heat up for 2 layers of 3mm glass:

240C/hr to 250C, no soak

400C/hr to 500C, no soak (a bubble squeeze could be inserted here by raising the target temperature to 650, with a 30-minute soak)

500/hr to top temperature.

This is about 2.3 hours to top temperature without the bubble squeeze and 6.7 hours to cool.  This means that you could fire twice in one day, if organised well.  If you are planning a final tack fused layer that should be done in the last firing of the combined layers.

However, it is a much longer schedule recommended by Stone for 6 layers of 3mm glass:

• 25C/hr to 125 for 20’
• 30C/hr to 250 for 20’
• 40C/hr to 375 for 20’
• 50C/hr to 520 for 15 (a bubble squeeze could be inserted here by raising the target temperature to 650, with a 30-minute soak before continuing at the same rate to the top temperature).
• 150/hr to target temperature

This is about 18 hours to top temperature without the bubble squeeze and another 18 hours to cool.  This strategy requires 1.5 days, assuming all the layers are even.  The same amount of time is required for both strategies, but the chance of large bubbles is dramatically reduced.

He recommends for 3 layers of 6mm glass:

• 200C/hr to 250, no soak
• 340C/hr to 500, no soak
• 400C/hr to 600, no soak (a bubble squeeze could be introduced here by changing the target temperature to 650 with a 30-minute soak)
• 500C/hr to top temperature.

This is about 2.5 hours to top temperature and 18 hours to cool without the bubble squeeze.

This means that it only takes 2/3 of the time to fire 3 layers of 6mm glass than it does to fire 6 layers of 3mm glass.  Yes, you lose some time in firing the pairs of 3mm glass, but you gain in reducing the risk of creating large bubbles that will ruin your final piece.

Inclusions

If you are putting elements between the initial two-layer pieces for fusing, you need to introduce a bubble squeeze.  Putting elements between the fused pairs will also require a bubble squeeze on the final firing.

Tack fusing the final layer

Note the times indicated above are for even layers.  If you have uneven layers or are tack fusing, the times will be extended much further than the ones noted there.

For a tack fused set of top layers, you will need to add those in the last firing, or do a sharp tack firing before the last firing.  In the case of a tack fused pair for the top layers you will need to reduce the rates of advance for the last firing by about 1/3. This would mean:

• an initial rate of 135C,
• a second ramp of 230C,
• a third of 270C and
• the fourth of 335C instead of the rates for even layers. 

You will also need to reduce the top temperature.  Observation will be required to determine when the correct profile has been achieved.

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

When firing multiple layers of glass, the risk of creating large bubbles can be reduced by firing pairs of 3mm sheets, and then combining the results into one stack.

*Graham Stone. Firing Schedules for Glass, the Kiln Companion, 2000, Melbourne Australia.  ISBN 0-646-39733-8

Expansion at Edges of Tack Fused Stacks

How much will my glass expand if I put glass pieces on top of 6mm base?  

I ran some tests for both 6mm and 3mm bases. These showed that the distance from the edge is important.  The amount of glass in the stack has a big influence on expansion.  So does the tack profile and the thickness of the base.

The most expansion for any thickness and at any tack profile is when the stack is placed at the edge.  The further away from the edge, the less the expansion. There is no noticeable expansion of size when the tack stacks are placed 20mm from the edge.  In most cases there is only a little expansion at 10mm from the edge.  Although not tested, it seems that 15mm is a safe distance from the edge to avoid changing the edge.

The amount of glass in the stack being tacked to the base has an effect on the amount of expansion.  This is to be expected based on the concepts behind volume control.  Two tack layers can vary from two to three times that for a single tack layer depending on the profile of the tack.

The tack profile has an effect on the amount of expansion.  At contour there is a greater expansion than at rounded or sharp tack fuse.  This is to be expected, as there is less heat work at sharper tack profiles than at contour.

The thickness of the base has an influence on the amount of expansion too.  Thicker stacks promote greater deformation of the edge at all tack levels.  Thicker stacks need to be placed further from the edge to avoid changing the perimeter.  Thicker stacks create greater change in the edge on single layers than double layers.

The setup and results are given here.

Setup for 2 layer base and 1 and 2 layer stacks at various distances from the edge.

Contour fuse test, 6mm base
1 layer placed at edge, at 10mm from edge, at 20mm from edge, and at 30mm from edge.  2 layer stacks placed in the same way.  
 

Fired results, outlined for clarity

1 layer placed at edge – expansion of 2.5mm
1 layer placed 10mm from edge – expansion of 0mm
1 layer placed 20mm from edge – expansion of 0mm
1 layer placed 30mm from edge – expansion of 0mm

2 layers place at edge – expansion of 9mm
2 layers placed 10mm from edge – expansion of 2mm
2 layers placed 20mm from edge – expansion of 0mm
2 layers placed 30mm from edge – expansion of 0mm
 

Rounded tack test, 6mm base
1 layer placed at edge, at 10mm from edge, and at 20mm from edge.
2 layer stacks placed in the same way.
 
1 layer placed at edge – expansion of 3mm
1 layer 10mm from edge – expansion of 0mm
1 layer 20mm from edge – expansion of 0mm

2 layers place at edge – expansion of 7mm
2 layers placed 10mm from edge – expansion of 1mm
2 layers placed 20mm from edge – expansion of 0mm
 

Fired result of 6mm base with 1 and 2 tack layers, rounded tack.

 
Rounded tack test, 3mm base
1 layer placed at edge, 1 at 10mm from edge, 1 at 20mm from edge, 1 at 30mm from edge.  2 layer stacks placed as above.  
 
1 layer placed at edge – expansion of 2.5mm
1 layer 10mm from edge – expansion of 1mm
1 layer 20mm from edge – expansion of 0mm
1 layer 30mm from edge – expansion of 0mm
 
2 layers placed at edge – expansion of 3mm
2 layers 10mm from edge – expansion of 1mm
2 layers 20mm from edge – expansion of 0mm
2 layers 30mm from edge – expansion of 0mm
 

Fired result of 3mm base with 1 and 2 tack layers.

Note: the single 200mm sheet contracted to 195mm in uncovered areas.  Measurements were based on the amount of expansion from the fired dimensions. Even with the greatest expansion the piece was still 2.5mm smaller after firing than at the start.
 

Sharp tack test, 6mm base
1 layer placed at edge, 1 at 10mm from edge, 1 at 20mm from edge, 1 at 30mm from edge.  2 layer stacks placed as above.  

 
1 layer placed at edge – expansion of 1mm
1 layer 10mm from edge – expansion of 0mm
1 layer 20mm from edge – expansion of 0mm
1 layer 30mm from edge – expansion of 0mm
 
2 layers placed at edge – expansion of 2mm
2 layers 10mm from edge – expansion of 0mm
2 layers 20mm from edge – expansion of 0mm
2 layers 30mm from edge – expansion of 0mm
 

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

Firing Uneven Layers

There are a number of people firing stacked layers of glass in a pyramidical fashion to melt the layers down, in a nod to the 1950’s.

Annealing of a full fused platter of this nature is easier than a tack fused one. The degree of contour still in evidence will be important in determining what the annealing schedule should be.

Full or Tack Fuse

In this example shown by Vicki Urbich there are at least four layers - five if the base is two layers, although in this case there is only one.  A full fuse at 800°C will not be enough to give a flat piece for a trivet or platter.  You could extend the soak at 800°C but, it is better to go to 816°C for ten minutes rather than an extended soak at lower temperatures to avoid devitrification.

Damming

The edges of this piece will be wavy, unless dammed, because of the uneven layering.  Placing dams around will give crisp edges to the piece, even though the stacked pieces will round and spread. 

Annealing stacked pieces

Anneal this set-up for at least 9mm for a full fused piece. The pieces will spread and attempt to fill the gaps between the stacks.  Even with an 816°C fuse, the pieces will not be perfectly even in thickness.  To be safer, and account for the remaining unevenness, anneal as though it were 12mm thick.  Other lay-ups will have slightly different requirements.

If it is to be tack fused, you will need to anneal considering the different thicknesses across the piece.  You will have nearly 12mm thick at the thickest and only 3mm at the thinnest.  The generally accepted recommendations are to anneal for twice the thickest part - 24mm in this case.

The anneal is more than the length of soak. It is a combination of the soak and the rate at which you cool to at least 370°C. The cooling rate is directly related to the length of the soak.  If you require twice the length of soak at the temperature equalisation soak, you will require half the speed of anneal cool.  The Bullseye Chart forAnnealing Thick Slabs will give you the relevant rates regardless of the glass you are using. The temperature points will change for other glasses, of course, but the rates remain the same.

Rate of Advance

The earlier problem this lay-up gives you is the heat up to avoid thermal shock. 

The heat up of 4 layers of glass stacked on a single or even two-layer layer base is more difficult than for even layers across the whole piece. Each upper piece shades the heat from the lower ones, making for cool and hot areas next to each other.  With four layers, each layer needs to heat through to transfer its heat to the one below.  This means the bottom of the stack will take a long time to become as hot as the top layer.  Meanwhile, the uncovered glass is getting as hot as the top of the stack.  This often leads to the bottom layers breaking from the stress of the uneven heating.  

Graham Stone suggests 100°C (180°F) per hour for four, even layers. As this is four uneven layers, the rate of advance should be at least half that. This should be used all the way up to the bottom of the bubble squeeze to allow all the glass to heat at the same rate. Glass generally reacts better to a slow, steady contant rate of advance in heat, than faster rates with multiple soaks.

Bubble Squeeze

The bubble squeeze for this single layer base piece can be as quick as 50°C per hour over the 50°C range.  It does not need to be slower, as the weight of the stacks pushes the air out between layers more quickly than large, even and lighter layers.  A double layer base requires a slower bubble squeeze because the weight of the stacks will push the air out to be between the two base layers.  This means a rate of 30°C or even 25°C through the range.

Then you can go faster to the top temperature.

Firing uneven layers requires extreme care on the initial heat up to avoid thermal shock.  A high fusing temperature is needed to get an even thickness across the piece.  Annealing is easier to calculate for even pieces, but must be much more cautious for tack fused items.

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

Large Bubbles

As you move up from smaller pieces to pieces that occupy most of the shelf, you sometimes begin to get large rounded bubbles at tack fuse and burst ones at full fuse.

Image from B Stiverson

You have to go back to basics to discover the cause.

Schedule

It is not likely to be the schedule. It has worked for smaller items. But it is important to review the schedule.  Is it like others you have seen? Is it similar to what the glass manufacturer recommends?  Both these will reassure you that the schedule is OK, if not perfect, or to revise it.

Cleanliness

Going back to the basics relates to the cleanliness of your kiln, among other things.  Even a small speck of material under the glass can result in a bubble. Although the grit lifts the glass off the shelf only a fraction, as it heats up the glass slumps around that and creates an air pocket.  That grows as the glass heats up and creates a large diameter bubble. If there is no grit in evidence, you need to check another element of your kilnforming practice.

Shelf

The large bubble might often occur in the same relative place in the kiln, although different places on the glass pieces, depending where they are placed.  This is an indication that you may have a hollow in the shelf. It may not have been obvious with smaller pieces.  You need to check the shelf with a straight edge. If any light is seen between shelf and edge, you have a depression in the shelf.  It may only be a sliver of light, but that indicates a depression which is enough to create a large bubble. That must be fixed.

Image from Suze

There are temporary and permanent fixes for avoiding bubbles due to depressions in the shelf. 

The temporary fix is to use 1mm fibre paper on the shelf, to allow air out from under the glass.  This can be topped with Thinfire or Papyros. Alternatively, a thin layer of powdered kiln wash can be smoothed over the fibre paper to give the smoothest back possible in the circumstances. You can use a plasterer’s float, or simply a piece of float glass.

The permanent fix is to sand the shelf smooth and level.  A method for doing this is here.

Single Layer Bases

If you are firing with single layer bases, there may be nothing wrong with the shelf.  It is typical in tack fusing to use single layers with glass placed decoratively around the surface of the base.  This leaves gaps where the base glass is exposed.  Even though the whole piece may survive the differential heat up of the exposed base glass and the covered parts, there is the possibility of creating an air pocket under the exposed base.  This comes from the weight of the stacked glass pressing any air out to the side.  If the design is unable to provide a route out for the air, the possibility of creating an air bubble increases.

It is possible to create conditions to reduce the possibility of these large bubbles developing. 

One solution is to use a layer of fibre paper as for a shelf with slight depressions.  This allows air out from under the glass, even with a single layer layup.

The other solution is to change the rate and temperature of the firing.  By using the low and slow principle, you can reduce the risk of bubbles.  Use a much slower rate of advance to a lower temperature with a longer soak you can achieve the look you want without bubbles.  This utilises the concept of heat work.  It does require observation to determine when the effect you desire is achieved and then advance to the next segment.

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

Tears in Slump

An enquiry was received about a tear in the slump of an intended bowl. It was reported that it was tack fused, giving a variation in thickness between 6mm and 9mm. The blank was tack fused with the following schedule: 

139°C to 560°C  30

222°C to  621°C  30

139°C to 786°C  15

9999  to  515°C  120

60°C   to 427°C  10

115°C to  350°C  10

This is a bit odd, as it had a slow rate of advance to top temperature and no bubble squeeze. But it should not have been a problem for this piece.

It was then slumped. When the kiln was opened after the completion of the slump, this split was revealed in the centre of the bowl, rather than a complete break.

The schedule was again a bit odd and high:

83°C to  148°C  15

167°C to  590°C  10

83°C   to 720°C  10

222°C  to 410°C  120

83°C    to 427°C  10

The very slow start would protect against any heat shock, but the schedule doubled the rate of advance while the glass was still in the brittle phase.  This possibly induced some stress into the glass.  There is no reason why the rate of 167°C per hour could not have been continued to about 630°C to 640°C.  There is no need to slow the rate of advance once the glass is out of the brittle phase (ca. 540C).  With this slow rate of advance, the bowl may have been slumped into this simple ball mould at 620°C or less.  

This indicates that observation is needed when trying new layups and moulds to find the appropriate temperature.  It reveals at what stage any problem occurs.

There are several possibilities to consider in diagnosing the failure of this piece.

Rate of advance 
It might have been just too quick for the thickness of the piece. The piece is reported to have varied from 6mm to 9mm. From the picture this might have meant a single layer base, or more likely, a two-layer base and then the two-layer top pieces, making it 6mm to 12mm.  The firing schedule would need be as for an 18mm piece in the first instance, and 24mm in the second.

The initial rate of advance is more than slow enough for the calculated size of the thickest. The doubling of the rate of advance in the early stage of the brittle phase of the glass is more problematic. It may have had the effect of inducing a weakness (stress) that became apparent in the next segment with a slower rise to the top temperature. It probably heated the top much more than the bottom during this second segment, leading to the tear.

Was it adequately annealed?  
If you look at the fusing schedule, the anneal soak and anneal cools were adequate for a 12mm piece, so if compatible glass was used, there should be no annealing stress in the piece.  It is important to consider this, as a stressed piece can often break during an otherwise adequate slump schedule.

The placing of the piece may have had a significant effect on the outcome.  It is placed in the corner of the kiln.  A single element shows around the side of the kiln.  This would not be enough to heat the whole kiln, so we must assume it is mainly top fired. If the kiln has significant differences in temperature (only as much as 5°C), the location in the corner may have had enough of an effect to cause the stress.

When did the split occur? 
It is possible that the split occurred on the way up and then re-attached during the slow rise to the high working (lamination) temperatures.  This would give the appearance of an incomplete split, commonly called a tear.  We don’t have any information about the state of the edges. At 720°C an early split could have re-attached. The reason for considering this possibility, is the change of curve on the left end of the split. However, this does not seem likely as the split clearly shows on the edge of one of the squares, but does not go all the way across.  Lamination temperatures are not high enough to seamlessly heal a crack.

It is most likely the split occurred during the rise in temperature.  The reason for speculating this, is because of the distortions of the squares.  If the split occurred before any significant slumping the distoritions in the squares would be explained.

Range of Considerations

This discussion shows that there is much more than just the schedule to consider in diagnosing failures. 

Yes, the schedules are odd, but not impossible to get a good result with.  The fuse and slump schedules vary to a large extent which is not ideal.  

The fuse schedule to the bubble squeeze temperature is sensible, but the slow rate of advance is continued to the top temperature, which is not usual.  This means there was no consideration of a bubble squeeze soak, although this did not prove to be a problem. The annealing is suitable for up to 12mm.

The slump schedule starts very slowly and then doubles early in the schedule.  This rapid change of rate early in the brittle phase of the glass may have induced stress that could not be relieved later in the firing. A simple single rate of 167°C to the slumping temperature would have been adequate. 

The slump temperature used is in the lamination/sharp tack range, rather than the more usual 620°C to 677°C range.  This can bring several problems with excessive marking of the bottom of the piece, shrinkage, and even uprisings at the bottom of the piece.

Are any of these criticisms of the schedules adequate to point to as causes of the break? Without handling the piece, it is difficult to tell with the information available.

General Diagnosis

You need to consider the state of the break in diagnosis.  We do not know whether the edges were sharp or slightly rounded. It is clear the split piece fits the mould as it is, so the break probably occurred on the way up in temperature.

Was the high slumping temperature an element in the break? The third rate of advance was slow, so there should be no further stress introduced in the firing.  The annealing of the fused piece seems adequate, so a stress fracture does not seem likely.

The high slumping temperature may be disguising a problem, as the glass may have re-attached at the upper temperature.  But this does not seem likely as the picture seems to show the crack enters the red piece a short distance, but not all the way through.

Was the placing of the mould problematic? It is in a corner where there may be enough difference in temperature across the glass to induce this kind of tear.

These considerations show that multiple images of a problem piece need to be taken.  Various angles are required to eliminate problems with reflections.  Pictures of the whole setup in the kiln and the piece are needed.  Multiple pictures of the top and bottom are needed. And of course, close ups of the area(s) concerned.  These are all substitutes for handling the piece itself.  

If you have a community of kilnformers or a store you can take the piece to, you are likely to be able to give responses to questions and to get the information required about the possible problems and solutions.

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