Inadequate Annealing - Effects on Next Firing

Credit:

https://immermanglass.com/about-kilnforming/cracks/

The speculation about breaks caused by inadequate annealing of the piece on the previous firing is common.  I do not know if this can be proved to be inaccurate, but we should think about it.

A parallel condition to this poor annealing is toughened/tempered glass which is under a lot of stress between the inside and outside surface of the glass. As Bob Leatherbarrow mentioned to me, we can heat up the highly stressed toughened glass without breaking it by using moderate ramp rates. During this heat up in the brittle phase, the stress is gradually relieved. It does require the moderate ramp rates, of course. 

This parallel circumstance of heating toughened/tempered glass which is highly stressed raises the question: Why should mildly stressed kilnformed glass suffer breakage, if fired at a reasonable rate? Highly stressed toughened/tempered glass does not.

If we apply the experience of relieving the stress in toughened/tempered glass, you can see how inadequately annealed glass behaves. The under-annealed glass has stress distributed (possibly unevenly) across its substance. As the glass temperature moves toward the strain point it becomes less brittle and the stresses are reduced. By the time the glass reaches the strain point, the stresses from poor annealing are relieved.

Any glass not fired slowly enough for its thickness or layup toward 300˚C/573˚F will break. This has been observed to occur around 260˚C/500˚F.  This most commonly occurs in pieces that are laid up with different thicknesses  across the surface. The heat cannot reach the bottom layers as quickly as the overlying ones. The expansion of covered and uncovered glass - due to the heat exposure - is to different.

Thinking about the behaviour of glass in this way indicates that breaks early in the firing relate to a too rapid ramp rate, not necessarily a previous annealing problem. We should, of course, be checking on the stress in our pieces after each firing. This will alert us to the amount of stress in the piece and so to be more cautious in the ramp rate and in the annealing during the current firing. 

Speculation about inadequate annealing in a previous firing as a cause of breaks is misplaced. The thinking that stress will carry through the heat-up and cause breakage is misdirected. 

More information on this is available in the eBook LowTemperature Kilnforming, an Evidence-Based Approach to Scheduling at Etsy VerrierStudio shop and from Bullseye Ebooks.

Refiring and Annealing

A question about re-fusing was posted:

 I have just taken a large [rounded tack] piece, with … A small piece … flipped and showing the white side…. If I cover this with a thin layer of coloured powder frit, does the piece need the long anneal process when I fire it again... I will be taking it up to the lowest tack fuse temperature possible, so the rest doesn’t change too much.

When considering the re-firing of a fused piece, even with minimal changes, the schedule needs re-evaluation of both ramp rates and annealing. 

Ramp Rates

Previously the piece was in several layers. The piece is now a thicker single piece and needs more careful ramp rates. You cannot fire as quickly from cold as the original unfired piece. Previously, the sheets could be heated as though separate. They were not hot enough to stick together until beyond the strain point. They could withstand the differential expansion that rapid heating causes. 

The thicker, previously rounded tack piece will need a slower initial ramp rate. Looking at Stone* and the Bullseye chart for Annealing Thick Slabs indicates the rate should be halved for each doubling of calculated thickness. A rounded tack firing of two layers should be fired as though twice its actual thickness. This means using a schedule for 12mm/.05” thick rather than 6mm/0.25”. This would be at a rate of 330°C/595°F. 

The first firing was of two layers of 3mm/0.125”. Now you are firing a tack fused piece of 6mm/0.25”. It requires a rate of 165°C/297°F as the first ramp rate. If you started with a rounded tack of two base layers and one tack layer, you may have been using a first ramp rate of 150°C/270°F (for 18mm/.075”). Now you will need to be thinking of 75°C/135°F as your first ramp rate. 

Annealing

The annealing time and cool rate will not be affected in the same way. In the first firing you are already annealing for the two layers forming a single piece of 6mm/0.25”. As there is no change in the profile or thickness of the piece, it can be annealed as previously. The cooling rates are the same as for the first firing. 

Credit: Bullseye Glass Company

Refiring with Additions

Ramp rate

If there are additions to the thickness, a slower ramp rate will be required. For example, if an additional 3mm layer is placed on top of a 6mm/0.25” base for a full fuse the ramp rate will need to be reduced to that for 9mm/0.375”, i.e., 415˚C/747˚F according to various charts. However, I never fire faster than 330˚C/595˚F.  There is too much risk in breaking the glass through differential expansion with fast rates.

 

In this case the firing is for a rounded tack. You will need to schedule as for 18mm/0.75”. The rationale for this doubling of the thickness is in my ebook Low Temperature Kilnforming. This initial rate for 18mm/0.75” will be 150°C/270°F. 

Annealing

This time the annealing will need to be longer than the first firing. The thickness has changed with the additions of pieces for a rounded tack firing. Instead of annealing for 6mm/0.25” you will be annealing as for 18mm/0.75”. This requires a hold of three hours at the annealing point and cooling over three stages. The first two of these stages are 55°C/100°F each. The first cool rate is 25°C/45°F per hour and the second is 45°C/81°F per hour. The last is at 90C°C/162°F per hour to room temperature. 

These examples show how dramatically later additions in thickness can add to the length of the firing to get a well-annealed piece without breaking it on the heat-up. 

 

*Graham Stone. Firing Schedules for Glass; the Kiln Companion. 2000, Melbourne. ISBN 0-646-397733-8

As a side note, Stone’s book has become a collectable.

 

The Mechanism of Sintering

 "Do glass molecules actually migrate when they are sintered together? "

Sintering occurs at the atomic level, where the atoms at the edge of the particles attach to others in other particles. An analogy occurs to me of Scottish country dancing. In big gatherings, small groups are formed to perform the dance, say an eightsome reel. As the dance goes on the groups become more coordinated and eventually form one large group, held together by the people on the edges of each group.

A more scientific description comes from Wikipedia:

“Sintering … is the process of compacting and forming a solid mass of material by heat or pressure without melting it. … 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.”

Applied to glass this means that you can make a solid piece of glass out of multiple touching or overlapping pieces that do not change their shape. This uses low temperatures and very long soaks.

 Schematic-diagram-for-the-sintering-and-fusion-reaction-of-the-glass-frits-on-a-substrate.
Credit: ResearchGate

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 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 atoms of the molecules time to combine with their neighbours in other particles.

Sintering occurs in the range of 610°C to 700°C (1130°F to 1275°F). The lower limit is determined by the strain point of the glass and by practicality. The length of time required at the strain point - 540°C/1005°F - is so long (days) that it is impractical.

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. The process of crystallisation breaks the bonds already formed between the atomic structures of the molecules. These studies showed that the onset of devitrification is at 650°C/1204°F and is visibly apparent at 700°C/1292°F regardless of the glass used.

The lowest practical temperature for sintering is 650°C/1203°F. Indications are that at least an additional two hours are needed for the sinter soak for each 10°C/18°F reduction below 650°C/1203°F. This would make for a 12-hour soak at 610°C/1131°F. For me this is not practical.

More information on the kilnforming processes and sintering experimentation is available in this eBook: Low Temperature Kiln Forming.

Effect of Air Space Around Shelves

The Bullseye research on annealing thick slabs indicates that it is important to have a 50mm space between the shelf and the kiln walls. This is to assist even distribution of the air temperature above and below the shelf.

I decided to learn what the temperature differences are between ventilated and unventilated floors of kilns. The recording of the temperatures was conducted using pyrometers on the floor of the kiln and in the air above the kiln shelf. The pyrometer above the shelf was at the height of the kiln’s pyrometer. The recording was done during normal firings of glass. The graph below shows temperature differences during a typical firing.

The blue line indicates the air temperature, the orange line the floor temperature and the grey line the difference in the two over the whole firing. Each horizontal line is 100C

The next graphs show in more detail the differences between having no significant space and another firing with space between shelf and kiln walls.

Horizontal axis legend:

1.  = 300°C
2.  = Softening point
3.  = Top of Bubble Squeeze
4.  = Top temperature
5.  = Start of anneal soak
6.  = start of first cool
7.  = start of second cool
8.  = start of final cool
9.  = 300°C
10.  = 200°C
11.  = 100°C
12.  = 40°C

The general results are that there is a greater difference during the rise in temperature and a reducing difference in floor and air temperature during the anneal cool. However, there are significant differentials at various points during the firings.

Space between the shelf and kiln walls:

• Smaller temperature difference is experienced on the heat up.
• Floor stays hotter than the above shelf air temperature during the anneal soak.
• This difference gradually equalises during the anneal cool

Without space between the shelf and kiln walls:

• Significantly greater difference on heat up is experienced – over 100°C cooler than ventilated floor area.
• Floor temperature is less than air until the final cool.
• During the anneal soak the floor temperature difference becomes larger than at start of anneal. This seems to be the consequence of heat continuing to dissipate through the kiln body, while the air temperature above the shelf is maintained at a constant temperature.
• The difference between the air and floor temperature gradually reduces during the anneal cool as the whole kiln and its contents near the natural cooling rate of the kiln.

 

This appears to indicate that space between the shelf and kiln walls helps to equalise the temperature during the critical anneal soak and first stage of the anneal cool. This will be particularly important when annealing thick slabs.

These tests were done in a kiln of 50cm square. It is likely that the differences would be greater in a large kiln, making it more important to have the air gap between shelf and kiln wall. Smaller kilns and thinner glass seem to be less affected by these differences.

Note that the air temperature and shelf temperature differences in these firings maintain the same character whether the floor has good circulation or not. The shelf temperature lags behind the air temperature throughout the heat up.

The fact is that floor and air temperatures are nearer each other with air space around the shelf. The difference reduces during the bubble squeeze and the top temperature soak. The difference in temperature on cool down is small. During the anneal soak and cool, the shelf tends to be a few degrees hotter than the air temperature.

There was no difference in the amount of stress in the glass in these tests on a small kiln whether there was a gap or not between the shelf and the kiln walls.

Implications for kilns with multiple shelves

Those using multiple shelves in a single firing load should take note of the implications from this. It is important to have significant ventilation between layers to get consistent results from firings.

The ideal would be to have larger than 50mm/2” gap around the upper shelf. Possibly 100mm/4” would be a good starting point. This would allow sufficient heat circulation to compensate a little for the lack of radiant heat from the elements.

If you have a really deep kiln and are using three shelves, the ideal would be to start with a 50mm/2” gap around the bottom shelf. Then a 100mm/4” gap around the middle shelf and finally a 150mm/6” gap around the top shelf. This will assist the heat to circulate to the bottom layer.

 

There are greater differences in temperature between the floor and above shelf air temperature when there is no ventilation space around the shelf. This is especially the case during the anneal soak.

Longer Anneal on Each Firing

 Need for an Extension of Anneal Soak on Subsequent Firings

 Sometimes people recommend extending the length of the anneal soak each time the piece is fired. If nothing significant is added, there is no reason to extend the anneal soak.  If the piece can be fired as fast as the previous firing, the annealing will be the same, not longer.

 The physics and chemistry of annealing glass are the same for re-fired glass - without additions - as they were for the first. Extending the annealing soak seems to be more about reassurance of the kilnformer than a necessity.

 Bullseye research has shown that it IS possible to over anneal, locking in stress. If concerned about inadequate annealing, it is best to reduce the cooling rate. Especially over the first 55°C below the anneal soak temperature.  The testing and recording that I have done for a book on tack fusing shows that any differences in the glass - at the end of the anneal soak - will be relieved in that first 55°C/100°F. The remainder of the cool to 370°C/700°F can be about 1.8 times faster, and the final cool ramp can be 3 times faster than the 2nd stage cool. 

 I have observed that a three stage anneal cool is important to successfully anneal a piece. This has been reinforced by the temperature recordings of many firings. Often at the end of the anneal soak there is a little more than the desired 5°C/10°F difference in temperature across the piece. The recordings show this is relieved during the slow firs stage cool and maintained over the next two cool stages. If the kiln is cooling more slowly than the schedule, no electricity is used.  No kiln time is lost.

An example of the first cooling stage

 The first stage cool is key to a successful stress-free result.  If there are concerns about inadequate annealing, two things are important.  Be sure the right length of soak is chosen for the piece being fired.  Second, reduce the speed of cooling by the rates for a piece at least 3mm thicker.  These rates are available from the Bullseye chart for annealing thick slabs.

 The rates are applicable to other than Bullseye glass.  Only the temperatures need to be changed.

 If no significant changes (other than powder, wafer or stringers) are made to the glass before the second firing, no lengthening of the annealing is necessary.

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

Texture Moulds

 Texture moulds are a form of bas relief in reverse. The texture of the mould is the bas relief. The glass formed over the shapes is in negative relief. The light is refracted through th
e back to give an image of bas relief although the surface is smooth.

 

Example of wave form texture mould

 These moulds are prone to produce bubbles at the generally recommended tack fuse temperatures. The glass often sticks to the mould if there is not sufficient draft to the parts of the image, or if insufficient separator is used. Often the moulds are produced with a rim around the edges, which trap the glass.

 The usual temperatures are too high. These moulds are an exercise in patience. The temptation is to fire higher than slumping temperatures to get good definition in the glass. However, a number of problems, especially bubbles, can be avoided by staying at the high end of slumping temperatures. This means the top temperature would be about 680C. To compensate for this low temperature, the soak needs to be three hours or more. To be sure the definition desired has been achieved, peeking near the end of this long soak is necessary. 

 Moulds that are produced with a rim around the edges can trap air and create bubbles. The rim forms a perimeter dam to confine the glass. If the rate of rise is quick to a high temperature, the edges can be sealed against the rim before all the air has escaped. It is advisable to cut the glass for these rimmed moulds a bit smaller than the internal dimensions formed by the rim.

 

Example of textured area surrounded by a rim

 Use of single layers on texture moulds can lead to large, thin bubbles. This is most prevalent when using high temperatures. Since the single layers tend to form more slowly than an already fused two-layer piece, the temptation is to use higher temperatures. The higher temperatures soften the glass to such an extent that often bubbles form over the lower areas of the mould. Instead, low temperatures with extremely long soaks should be used to allow the glass to conform to the undulations of the texture without dog boning or developing bubbles. Of course, peeking will be required to determine when the texture is achieved. With single layers, the surface will have greater undulations than with two layers. The thinness of the single layer cannot fill the depression the way two layers can.

 

 Rapid rates to high temperatures can produce internal bubbles too. These moulds have a multiplicity of hollows and depressions. Just as people are warned about depressions in their shelves, the depressions in the texture moulds can cause bubbles too. This means there are even more possibilities for bubble creation than on apparently flat shelves. Long slow bubble squeezes are required to allow air from under the glass.

 Glass sometimes sticks to the mould. This is most often blamed on insufficient separator. Boron nitride is a good separator for these moulds especially if you go to tack fusing temperatures. At slumping temperatures, kiln wash will normally be sufficient. Both of these separators need to be applied carefully, as there are relatively steep slopes throughout the mould. Spraying needs to be done from at least four angles to ensure all the sides are covered.

 Painting on kiln wash is a little more difficult, as the solution is so liquid, it tends to run down the slopes without much sticking. One means of rectifying this is to tip the mould in a circular motion to move the still liquid kiln wash solution around the slopes.

 Less often thought about is the draft of the shapes of the mould. If the slopes (draft) in the mould are too steep, the glass will “grab” the ceramic mould, because the ceramic contracts less than the glass when cooling. If shapes of the mould are steep and deep enough, the glass may even break as a result of this compression of the mould.

 

An example of some nearly vertical elements and a rim

 Of course, if a flat front surface is required, a higher than slumping temperature must be used. This is required to allow the glass to flow to the lower portions of the mould. It still should be as low as possible, but with very long soaks.

 Avoidance of bubbles on, and sticking to, texture moulds is best achieved by avoiding high temperatures, use long soaks, use two layers, and avoid extending glass to the rim. These combined with observation of the progress of the firing will produce the best results.

 

Other information is available:

Low Temperature Kilnforming, an Evidence-Based Approach to Scheduling, an ebook

Bas relief

Layups promoting bubbles

 

Sintering Ramps and Soaks

Sintering (or laminating) is a special form of low temperature kilnforming that requires attention to the ramp rates and the length of soaks. The rates and soak times were determined by the strength of the resulting pieces.

Credit: Researchgate.net

Rate

 The ramp rate has a significant effect on the strength of the resulting piece.

 A moderate rate (150°C/270°F) all the way to the sintering temperature of 690°C/1080°F gives the glass particles time to settle together. It works similarly to a slow ramp rate in slumping.

 A rapid rate (600°C/1275°F) - as used in medicine – to the sintering temperature of 690°C/1080°F is used for float glass particles.

 An alternative to both these is to schedule a rapid rise to the strain point followed by a slow - 50°C/90°F per hour - rate to the sinter temperature.

Soak

The soak time is extremely important in sintering to provide strong results. It is loosely related to the ramp rate, but in an inverse manner. The quicker the ramp, the longer the soak required.

 The moderate rate of 150°C/270°F needs a two-hour soak at the top temperature for maximum strength.

 The rapid rate of 600°C/1275°F requires about six hours of soaking at the top temperature.

 The alternative of a rapid rise to the strain point followed by the slow 50°C/90°F per hour rate requires at least a three-hour soak.

 These results show the ramp rate is important to the strength of the resulting piece. Fast ramp rates require increasingly long soaks at top temperature. Even slowing the ramp rate after reaching the strain point requires longer soaking than a steady rate. This is so even though the steady rate is faster than the two-part schedule to the top temperature.

 These results indicate that heat work is put into the glass throughout the temperature rise. The heat put slowly into the structure below the strain point still has an effect on the sintering of the glass.

 This is shown by the two-part schedule that has a slow ramp rate after the strain point. And even then, the time required is only 0.3hour shorter than for the moderate steady rise and soak. 

There is no time advantage to rapid rises to the strain point followed by a very slow rise to top temperature. The six-hour soak required by fast rises to top temperature show there is a large time disadvantage with rapid rise scheduling of sintering.

More information is available in the ebook Low Temperature Kilnforming and from Bullseye.

The Importance of Three-Stage Cooling

It is common to think of cooling after annealing as a simple single cool rate to an intermediate temperature between annealing and room temperatures before turning off. This most often works well for full fused pieces up to 6mm/0.25. But as the pieces become thicker or more complex, the need for more controlled cooling becomes necessary.

 The aim of annealing is to get the glass to be the same temperature throughout its substance during the annealing soak. This is called the ΔT (delta T).  This difference has been shown to be 5°C to avoid high levels of stress.  Therefore, ΔT=5°C/10°F.  This difference in temperature needs to be achieved during the annealing soak and maintained during the cool.

 The object of controlled cooling is to maintain this small difference in temperature. It needs to be maintained throughout the cool to avoid inducing excessive stress in the glass, even if the stress is only temporary.  

 As the thickness or complexity of the piece grows, the annealing soak needs to be longer and the cool slower. The first cool is critical to the production of stress-free fused glass. That is the fastest rate that can be used in a single or multiple stage cooling. If you use that rate all the way to 370°C/700°F you will need at least 1.3 times longer to get to that temperature than if you used the first two parts of a 3-stage cool. This time saving becomes greater as complexity and thickness demand slower cool rates. It is not only time that is saved.

 The risk of breaks from rapid cooling after the anneal soak and to 370°C/700°F increases with more complex and thicker pieces. Although the stress induced by rapid cooing below the strain point is temporary, it can be great enough momentarily to break the glass. This is so even if the glass meets the ΔT=5°C/10° during the annealing soak.

  

Examples may help understand the cooling requirements of glass that it thicker, or tack or contour fused.

Example 1

A 12mm/0.5” full fused piece needs a two-hour annealing soak, followed by three cooling rates of 55°C/100°F per hour, 99°C/180°F hour and finally 300°C/540°F per hour. The first rate is for the first 55°C/100°F, the second rate for the next 55°C/100°F, and the final rate is to room temperature.

 What happens here is instructive as to the reasons for soaks and cool rates. In this recorded example the ΔT at the start of the anneal is 7°C/12.6°F. During the soak, the ΔT reduces to as little as 2°C, but ends with a ΔT=3°C. The 55°C/100°F cool rate over the first 55°C/100°F enables the ΔT to remain between 3°C and 4°C.  The second cool over the next 55°C/100°F maintains this ΔT of 3°C to 4°C. During the final cool the ΔT varies from 5°C to 1°C.

 

An example of the variation in ΔT during the first 55C/100F of cooling

Example 2

A rounded tack fuse of 1-base and 2-layer stacks gives a total of 9mm/0.375”. Research has shown that you need to schedule for twice the actual thickness for rounded tack fusing - so for 19mm/0.75”.

This requires an anneal soak of 150 minutes, and a first cool of 20°C/36°F. The second cool rate can be increased to 36°C/65°F. The final rate can be at 120°C/216°F per hour to room temperature.

 The ΔT at the beginning of annealing was 7°C/12.6°F and at the end of a 2-hour soak was a ΔT of 1°C/2°F. The first cool ramp was 20°C/36°F per hour and gave a variance of between 2°C/3.6° and 0°. The final cool produced variances of up to 6°C/11°F, ending at 88°C/190°F with a ΔT=2°C.

 The first two stages of cooling save 1.27 hours of cooling time over a single stage cooling of 20°C/36°F to 371°C/700°F. It still keeps the glass within that ΔT=5°C. More importantly, the third stage cooling is able to keep the variance to between 6°C and down to 2°C.

 The natural (unpowered) cooling rate of my 50cm/19.5” kiln at 370°C/700°F is 240°C/432°F per hour. It settles to the 120°C/216°F per hour only at 200°C/392°F. This is a fairly typical cooling rate for medium sized kilns. This rapid cooling at 370°C/700°F creates a greater risk of breakage than the controlled cool.

 

An example of the ΔT during the second 55C/100F of cooling

Example 3

A sharp tack or sintered piece with two base layers and two tack layer stacks on top requires firing as though 30mm/1.18”.

 This needs a 4-hour soak during which the ΔT varied from 8°C to 4°C. The first cooling rate was at 7°C/12.6°F and gave a ΔT variance of 4°C to 2°C. The second cooling rate of 12°C/22°F produced variances of 3°C to 1°C by 370°C/700°F. The final cool of 40°C/72°F per hour gave differences ranging from 5°C to 0° at 110°C/230°F.

 Note that the test kiln’s natural cooling rate does not achieve the third cooling rate until 140°C/284°F.  This shows that turning off the kiln at 370°C/700°F produces a high risk of breakage for thick and complicated pieces.  In addition, the two stage cooling rates saves 3.27 hours of cooling time.

An example of the ΔT during the final stage of cooling to Room Temperature

 The temperature differentials below the strain point can exceed the ΔT=5. The stresses induced are temporary according to scientists. But they can be great enough to break the glass during the cooling. It follows that the anneal soak may have been adequate, but the cool was so fast that excess stress was induced by the differential contraction rates. This stress being temporary, implies that testing for stress in a broken piece may not show any. The momentary excess stress will have been relieved upon cooling completely to room temperature.  (IMI-NFG Course on Processing in Glass, by Mathieu Hubert, PhD. 2015 , p.9.)

 

More information on cooling is given in the book LowTemperature Kilnforming; an Evidence-Based Approach to Scheduling.

Frit Additions to Shaped Pieces

It is possible to stick frit to slumped pieces. But soaking for a long time – several hours - at 650°C/1200°F is required to stick the frit.  The added pieces will remain relatively sharp. You need to observe frequently from 600°C/1111°F to make sure that the form of the glass is not distorting. 

Credit: Pyramid Gallery, Smyth and Zebrak

Although it is possible, adding pieces to already shaped objects is not best practice, nor will it frequently give satisfactory results.  If the slump is shallow, it is more possible to do this successfully than steep or highly shaped forms.  But the most suitable practice is to flatten the piece, then tack fuse the pieces onto it. Follow this fusing with the new slump or drape.  This flattening process will not be possible with all shapes. 

The best results will be achieved by accepting what you have and make a new piece with the planned additions from the start.

This process will not be suitable for draped glass as the glass will drape further during this low temperature soak.

 

I've a book that gives more detail. Low Temperature Kilnforming, an evidence based approach to scheduling  or at Bullseye

Annealing Soaks are Related to Cool Rates

Good annealing is important to the success of each firing of a piece. 

This is generally agreed.

 

I do not understand the reasoning of those who use long anneal soaks followed by quick cool rates and early shut offs. I don't understand because reasons are not given. Or the reasons are in the realm of kiln fairies and other mythical beings.

The length of the annealing soak can be determined from established sources. The Bullseye table for annealing thick slabs gives the recommended soak times for evenly thick slabs of glass from 6mm/0.25” to 200mm/8.0”. Use that to determine the annealing soak time.

The soak times do not need lengthening except for pieces of uneven thicknesses. The ebook Low Temperature Kilnforming gives the calculations for variations in thickness and degree of tack. Generally, they are 1.5 for contour; 2 for rounded tack; and 2.5 for sharp/angular tack. Excessively long soaks are not desirable. This is additional evidence that long soaks and quick cools create problems.

The Relationship Between Soak and Cool Rate

Use of the Bullseye table shows that there are cool rates associated with the soak times. These rates for the length of annealing soak need to be used, as they are based on research, rather than fingers in the air or mythical beings.

My experiments have shown the need to control the cooling rates to at least 50C before shutting off. The end of an adequate annealing soak has the glass within 5°C/10°F of each other part (the ΔT=5). The slow cool for the first 55°C/100°F below is important to avoid exceeding that maximum differential. The rate for the next 55°C/100°F is faster and can allow a wider ΔT, as the stresses are temporary. But they can be great enough at any point to break the glass during fast cools. Therefore, the rates associated with the annealing soaks cannot be exceeded safely.

Do not just use "what works" for others. Use information based on research. The only company publishing research is Bullseye. Their research is applicable to all fusing glass with the appropriate temperature adjustments. 

If you use long annealing soaks and quick cool rates or ones that stop at about 370°C/700°F, you risk breakages of your glass. There is no reason to take that risk.  Also long cools from annealing to 370°C take longer than the staged cooling recommended by the Bullseye research.

 

More information is available in the ebook Low Temperature Kilnforming.

 

 

Breaks Early in Firings

 My pocket vases keep breaking underneath the fibre paper. What can I do?

If a pocket vase is going to break it most likely will be in the brittle phase of the glass. This is usually from too fast heating. It, more rarely, can be too fast cooling. This happens as the glass is moving from or into a solid.  It is an extreme case of shading heat from the lower layers.

The general condition

As the temperature rises, glass becomes a little less brittle. The viscosity of the glass reduces. This can also be expressed as becoming less brittle. Due to its excellent insulating properties, glass transmits heat slowly through its substance. This means that the expansion differences within the glass are greatest during the coolest part of the brittle phase.

The brittle phase is described as glass temperature being below the strain point. Then strain point is the temperature at which the glass exits the brittle phase. This temperature is about 540°C/1000°F for fusing glasses. It is higher for float and bottle glass.

The effect of shading heat from the lower parts of the piece is to induce different rates of expansion within the glass. The riskiest part of this temperature range is the lower part of the brittle phase. This is where the viscosity is highest and the rigid structure is easily broken by different expansion rates. This has been empirically observed by Bob Leatherbarrow and others to have greatest effect below 300°C/573°F. So, slow ramp rates are advisable to at least this temperature. Some continue this slow ramp rate to the strain point before increasing the rate.

 

Credit: Latta's Fused Glass

Pocket Vases

The effect of the differential expansion shows most obviously in pocket vases. This is a construction where fibre paper is inserted to create the pocket between two sheets of glass. This leaves the lower part of the glass under the fibre paper insulated from the heat. The other parts are left exposed to the radiant heat. While the exposed glass is getting hot, the covered glass is still cool. This sets up the conditions for the maximum differential in expansion rates. The differential in expansion causes the glass to break – usually it is the bottom piece that breaks. A major reason to schedule for at least double the glass thickness of a pocket vase is this shading effect. Slightly different calculations apply to tack fusing where there is no insulating layer between glass sheets.

The care in scheduling applies both to the first ramp rate and to the cooling rates of the fired piece. Fast cooling will leave the area covered by the fibre paper much hotter than the exposed glass. The difference in contraction can break the glass on the cool down too.

More information is available in the ebook Low Temperature Kilnforming; an Evidence-Based Approach to Scheduling. 

Achieving Multiple Profiles in One Piece

People ask about whether it is possible to tack fuse additional elements without affecting the profile of the existing piece.

It is as though glass has a memory of the heat it has been subjected to.  For example, a sharp tack will become a slightly rounded tack, even though refired to a sharp tack again.  So, it is impossible to refire a piece to the same temperature or higher without affecting the existing profile.  But it is possible to fire a piece with differing profiles if you plan the sequence of firings.

 

Tack fuse onto existing profile

 

It is possible to add pieces to be tack fused with little distortion to the existing piece through careful scheduling and observation.  There are several requirements.

 •     A moderate rate of advance to the working temperature is required, rather than a fast one. This is because the piece is a single thicker piece with uneven thicknesses.  Also, a slow rise in temperature allows completion of the work to at a lower temperature.  This means there will be less change to the existing profile.

•     A minimal bubble squeeze - or none at all - is required on this second firing.  The added pieces generally will be small, so if possible, eliminate the bubble squeeze.  The requirement is to add as little heat work as possible.

 •     The working temperature should be to a low tack fuse temperature with a long soak. 

 •     Observation is required from the time the working temperature is achieved.  Peeking at 5-minute intervals is needed.  This to be certain that the current tack fuse can be achieved without much affecting the existing profile.  It will be a compromise that you will be able to choose during the firing.  The decision will be whether to retain existing profile and have a sharp tack.  Or a slightly rounded tack and more rounded profile on the original piece.

Planning for multiple levels of tack

It is possible to design a piece with multiple profiles within the completed piece.  You need to plan out the levels and degrees of tack you want before you start firing. 

To do this planning, you need to remember that all heat work is cumulative. In simple terms it means that on a second firing you will start where you left off with the first one. The texture in the first firing will become softer, rounded, or flatter than the second or even the third firing.

Three degrees of tack can be achieved with a little planning.  It works similarly to paint firings.  Some paints fire higher than enamels, and enamels hotter than stain.  You have to plan to fire all the tracing and shading first.  Then you add the opaque enamels, followed by the transparent enamels.  Finally, you add the silver stain.  This is unlike painting on canvas where you build up the image all together.

The same principle is true of a multiple level tack fuse piece.  When creating various profiles in glass, you proceed from firing the areas that will be the flattest first. Then proceed to the areas which will have the least tack last.  This is a consequence of the cumulative effect of heat on re-fired glass.

Plan out the areas that you want to have the least profile.  Assemble the glass for those areas. I suggest that a 6mm base is the initial requirement for anything that is going to be fired multiple times.  Add the initial pieces that will become a contour fuse or a very rounded tack. 

First firing

Put this assembly in the kiln and schedule.  Do not fire to the contour profile temperature.  Instead, you will be scheduling for a sinter or sharp tack. This depends on how many textures you plan to incorporate.  Start with a sharp tack.  Fire at the appropriate rate with a bubble squeeze to about 740°C for 10 minutes and proceed to the anneal cool.   Different kilns will need other temperatures to achieve a sharp tack.

You do not fire to the contour fuse temperature, because the base will be subject to more firings.  Each of these firings will soften the base layers more than the previous one.  This is the application of the principle of cumulative heat work.  When you fire a piece for a second time, there will be little effect until the softening point of the glass is reached. Once there, the glass further softens, giving the effect of a contour fuse.

Any glass that had already achieved contour profile from the first firing will flatten further.  This can be used in cases where the working temperature was not high enough.  Just fire again to the original schedule’s temperature.  Take account of the need for a slower ramp rate to the softening point.

Second firing

Once cool and cleaned, you can add your next profile level of tack fusing to the base.  Note that “level of tack” does not refer to thickness being built up.  It is about the amount of roundness you want to impart to the pieces.  You may be placing this second - sharper – level of tack in the spaces left during the first firing.  Again, schedule to the original approximate 740°C. But remember the base is now a single piece.  You need to slow the ramp rate to the softening point, after which the speed can be increased.  You will not need to retain the bubble squeeze unless you are adding large pieces, or into low areas. 

The second firing will show the pieces added for the second firing to have the profile of the original pieces.  Those pieces having their first firing will have a sharper appearance.

 

credit: vitreus-art.co.uk 

This is a piece where the flower petals and leaves could have been placed for the second firing to give a softer background with less rounded flower details.

 

Third firing

Clean well and add the pieces for the final level of tack.  Schedule the initial rate of advance a little slower than the second firing.  The piece is growing in thickness and complexity.  Once the softening point is reached, the original rate of advance can once again be used up to original temperature. 

Final firing

Clean well and add the pieces for the final level of tack.  Schedule the initial rate of advance a little slower than the second firing.  The piece is growing in thickness and complexity.  Once the softening point is reached, the original rate of advance can once again be used up to original temperature. 

Further notes on multiple firings

It is a good idea to observe the firing, once the working temperature is achieved.  This is to ensure enough roundness is being given to the final pieces being tacked to the whole.  Be prepared to extend the soak if the final pieces are not rounded enough.   Although you should have a good idea of the degree of tack for the final pieces from the previous two firings.

You may need to experiment a little with the temperature and length of soaks at the working temperature.  For example, if the degree of tack is too sharp in the first firing, you can extend the soak or increase the temperature for the next ones. 

If you are firing at 740°C, you may feel you can afford to extend the soak for the subsequent firings, because you are in the lower part of the devitrification range. Consider the risk of devitrification increases with the number of firings of the glass.  The preference is to increase the temperature a bit for subsequent firings to ensure you are not spending a cumulatively long time in the devitrification range but still be able to get the final tack level desired. 

The preference is to increase the temperature a bit for subsequent firings to ensure you are not spending a cumulatively long time in the devitrification range but still be able to get the final tack level desired. 

Because most of your heat work is happening in the low end of the devitrification range, the cleaning regime must be very thorough.  Any chemicals or soaps used must be completely washed off with clean water.  The piece must be polished dry to ensure there are no water marks left on the glass.

You can, of course, have more levels of tack.  One approach would be to start with a sinter, or tack to stick, firing. And repeat that four or more times.  Another is to increase the working temperature and reduce the length of time soaked there.  The shorter time means there is less rounding of each level, allowing the build-up of many levels of tack.  All of these require some experimentation. 

More information is available in the ebook Low Temperature Kilnforming.

Three firings to the same sharp tack profile will give multiple profiles in the finished piece.