Home Made Billets

You can make your own billets from small pot melts.  But why should anyone go to the effort? Some reasons are:

• ·        You can make your own colour. 
• ·        You can use your cullet/scrap (avoiding buying or making frit).
• ·        You don’t have to buy and break billet to size 
• ·        You can reduce the clouding caused by many microscopic bubbles surrounding the frit pieces. 
• ·        You can make a size to fit your casting mould. 
• ·        Potentially, you will reduce needling.

 Now you are convinced of the advantages, you want to know how.

Preparation

• ·        Select the glass. Avoid iridised glass and any ground edges – they will cause haze in the final casting. Wash all the glass. Place the glass in a small flowerpot.
• ·        Weigh out the amount of glass cullet needed for the mould and add about 50gms to account for the glass that will stick to the pot.  Calculating the required weight is relatively simple and this post gives the information.

Dams

• ·        Arrange dams in such a way that the resulting billet will fit into the mould without overhang.  It might be quite a tall billet. In which case cast it horizontal with the height as the length of the billet.
• ·        Line the dams with Thinfire/Papyros at least. One mm fibre paper would be better. 
• ·        The dams can be on a kiln washed shelf or on fibre paper. The bottom of the glass will be fine either way.
• ·        Place the pot above the dams.  The higher, the fewer bubbles in the billet.  And any left in the billet will be reduced by flow in the casting firing.
• ·        Multiple billets can be made of different colours, sizes, etc., at the same time.

Firing

• ·        Fire to around 900ºC/1650ºF and soak for hours.  Observation will show when the pot is empty.  Clue: There will be no string of glass from the bottom of the pot.
• ·        Anneal as for the smallest dimension.  If you are doing multiple sizes, the dimension must be taken from the biggest piece.
• ·        When cool, remove and clean the separator off the pieces thoroughly.  A 15 minute soak in a 5% citric acid solution will speed the process.

Casting

• ·        Place billet in casting mould. The first ramp rate needs to be for the smallest dimension of the billet.  This may be a slower rate than when using frit for casting.
• ·        Do a long bubble squeeze in the 650ºC to 670ºC range – up to two hours, but a minimum of one.
• ·        Fire to your normal top temperature and time.
• ·        Anneal for the largest piece.

 

More information here 

Kilnforming Opalescent Stained Glass

The statement that a sheet of glass can be fused to itself is true in certain circumstances.  It applies to transparent and some streaky glasses best.  These forms of glass are more likely to fuse together successfully although not formulated for fusing.

Transparent and Streaky Glasses

Of course, the best practice is to test for compatibility.  I found in my early days of sticking stained glass together that it was beneficial to test. In doing so, I found Spectrum and Armstrong transparent and streaky glass to be largely consistent across many sheets.  I did not have access to much Kokomo or Wissmach.  I cannot comment on how their glass behaves in terms of compatibility across the production range.  Not all transparent and streaky glass remains stable at fusing temperatures. There are some glasses that opalise, some change colour, some devitrify. This variability makes compatibility testing important - even for the transparent form of stained glass.

Photo credit: Lead and Light

Wispy Glasses

The statement about fusing to itself is less applicable to wispy glass.  Not all the wispy stained glass from the same sheet can be fused.  It seems to be dependent on the amount of opalescence in any one area of the glass.  I found that it is possible - if you are very careful - to fuse certain Spectrum wispies with the clear fusing standard on top, but not on the bottom.  This should be applicable to other manufacturers’ wispy glass too.  There must be a marginal compatibility that is contained by the clear fusing glass on top, but I am not certain.

Photo credit: Lead and Light

Opalescent Glasses

The statement about fusing to itself is almost completely inapplicable to opalescent glass.  Stained glass opalescent glass does not have the compatibility requirements of fusing glasses.  They very often severely devitrify when taken to fusing temperatures.  This devitrification means that opalescent stained glass is often not compatible with itself.  So, no amount of twiddling with schedules will make stained glass opalescent glass fusible, even with itself.

Manufacturers have spent a lot of time and effort to produce fusing compatible opalescent glass.  It is as though there is a minor element of devitrification embodied in the opalising process.  Whether this is so, it becomes very apparent on doing compatibility testing that opalescent stained glass has severe devitrification at fusing temperatures.

Stock photo

Compatibility Testing

It is important to test for compatibility before committing to the main firing.  Some transparent and streaky glass changes colour, devitrifies, and some opalise at fusing temperatures. This applies with even more force to wispies.  They contain a significant proportion of opalescence within them.  Some opalescents are so unstable at fusing temperatures that the devitrification becomes so bad the glass crumbles.

The importance of testing pieces of the sheet for compatibility before committing to a firing is reinforced by these factors.

Slumping

Slumping temperatures are not so high as fusing, and it is often stated that single layers can be slumped.  Again, it is not always true.

Some glasses change colour at slumping temperatures.  A few opalise. It is not always certain what effect moderate temperatures will have on stained glass.  The compatibility testing will show.  Observe the test firing at slumping temperatures.  Also, you will learn if there are changes at moderate temperatures.

One element must be commented upon about slumping.  It is important to have the edges finished to the appearance that you want the final piece to have.  The regularity of the edges without bumps or divots, and the degree of polish need to be showing before the firing starts.  The slumping temperatures are not high enough to alter the shape or appearance of the edges.

Firing of stained glass to itself is normally a low risk activity, but with unpredictable results.  It can teach a lot about behaviour of glass at higher temperatures.  Slumping single layer pieces can give information about the way single layers of glass slump or drape.  But testing is important for fusing.  And can inform about how the glass will react at slumping temperatures too.

Testing your Scoring pressure

 Most often people are asked to listen to the sound of scoring.  Unfortunately, different glass styles make different sounds. Float glass makes a particular sound, transparent stained glass makes a slightly different one, and opalescent glass makes almost no sound. Consistent pressure of the right amount is important to the clean breaking of glass. Therefore, we must learn to cut with the same consistent pressure on all types of glass, rather than listening for sound.

It is easy to tell when the scoring is too heavy.  A white line shows along the score.

The heavy score line near the break shows the white line and the irregular break

It is not so easy to tell if the score is too light or just right.

A heavy score in the distance and a lighter score nearer

Pressure

The general recommendations for the pressure to use during scoring is 4.5 – 7 Lbs or 2 – 3 Kg. This is difficult to judge. I found that I needed a means of letting people know for themselves the pressure they were exerting. It is not enough to watch and say that was too hard, that was too soft, etc.

My method of teaching novices how to judge the pressure they are using is to use a digital kitchen scale that can have the scale set to zero. Place a piece of glass no larger than the platform on top of the scales. Zero the scale display.  Have someone watch the scale display while you score in your usual way. Of course, you must not touch the glass with your other hand. Have them tell you the maximum and minimum weights displayed. Keep repeating until you can consistently use that 4.5 – 6.5 pounds (2 - 3Kg) pressure.

The testing setup showing a heavy score on the right and the start of a 1.9kg score on the left.

Consistency

The other important element of scoring is to keep the pressure consistent throughout the score. This test will also show how evenly you apply the pressure during the score. The objective of scoring is to use the correct pressure throughout the length of the score. If your pressure varies significantly during the score, it will be difficult to get the glass to break consistently along the score line. Because the amount of weakness in the surface created by the score is variable.

Your observer can tell you when the pressure is less than optimum or more than desired.  If the pressure variation has a reasonably consistent place in scoring - such as at the beginning, or on a curve - you can fix it. Concentrate on correcting the fall off in pressure. For example, most people start off with a lighter pressure than further into the score.  Getting the feel of the correct pressure will enable you to apply it right from the start of the score. Sometimes, people increase the scoring pressure when they come to curves. This test will show if that is true for you.

This curve was scored with 4.3kg pressure showing that heavy pressure can result in break outs from the score line

This testing can take quite a while. But it is worth the time spent in getting the scoring pressure right to reduce the number of unwanted breaks. However, it is not a one-time test. When I begin to have difficulties in breaking glass, I go back to this test to check whether I am scoring too heavily. In my scoring practice, I find that my best ones are those with 1.8 to 2.5kg (4.0 to 5.5 pounds) with the cutter I use.  This is less than many, but it has worked well for me for years.

There are, of course, other elements that go to making a good score and break. But the most important thing in scoring and breaking opalescent glass is to avoid too heavy a score by listening for a sound. Cut to a consistent pressure whatever sound is heard.

 

Heat Up vs Annealing

I am amazed by the effort put into ramp up rates, bubble squeezes, and top temperatures in comparison to annealing.  The emphasis on social media groups seems to be to get the right ramp rates for tack fuses and slumps, bubble squeezes, etc.  Most of the attention is on the way up to processing temperature.

The treatment of annealing and cooling is almost cavalier by comparison.  The attention seems to be on what temperature, and how long a soak is needed.  Then some arbitrary rate is used to cool to 370ºC/700ºF.

Annealing, in comparison to firing to top temperature, is both more complex and more vital to getting sound, lasting projects completed.  Skimping on annealing is an unsound practice leading to a lot of post-firing difficulties.

Annealing is more than a temperature and a time.  It is also the cooling to avoid inducing temporary stress. That stress during cooling can be large enough to break the glass.  This temporary stress is due to expansion differentials within the glass.

People often cite the saving of electricity as the reason for turning off at 370ºC/700ºF.  My response is that if the kiln is cooling off slower than the rate set, there will be no electricity used.  No electricity demands.  No controller intervention.  No relay operation.

Annealing at the lower end of the range with a three-stage cooling provides good results.  The results of Bullseye research on annealing are shown in their chart for annealing thick items.  It applies to glass 6mm and much larger.  It results from a recommendation to anneal at the lower end of the annealing range to get good anneals.  Other industrial research shows annealing in the lower end gives denser glass, and by implication, more robust glass.  Wissmach have accepted the results of Bullseye research and now recommend 482ºC/900ºF as the annealing temperature for their W96.  The annealing point of course remains at 516ºC/960ºF.

Bullseye research goes on to show that a progressive cooling gives the best results.  They recommend a three-stage cooling process.  The first is for the initial 55ºC/º100F below the annealing temperature, a second 55ºC/100ºF cooling and a final cooling to room temperature.

It is a good practice to schedule all three cooling rates.  It may be considered unnecessary because your kiln cools slower than the chart indicates.  Well, that is fine until you get into tack and contour fusing.  Then you will need the three-stage cooling process as you will be annealing for thicknesses up to 2.5 times actual height.

 

Of course, you can find out all the reasons for careful annealing in my book "Annealing; concepts, principles, practice" Available from Bullseye at

https://classes.bullseyeglass.com/ebooks/ebook-annealing-concepts-principles-practice.html

Or on Etsy in the VerrierStudio shop

https://www.etsy.com/uk/listing/1290856355/annealing-concepts-principles-practice?click_key=d86e32604406a8450fd73c6aabb4af58385cd9bc%3A1290856355&click_sum=9a81876e&ref=shop_home_active_4

Slumping Strategy

A schedule was presented for a slumping problem of a 6mm/0.25” blank.  It consisted of three segments each of a rate of 277C/500F with short holds up to 399C/750F and then a rapid rise to 745C/1375F.  The cool was done with two long holds at 537C/1000F and 482C/900F followed by cooling rates for 12mm/0.5”

My response was that, yes it was fired too high.  Not only that, but the firing strategy, as shown by the schedule, is odd. 

Strategy

The general strategy for slumping follows these ideas.

·        Glass is slow to absorb heat, and in one sense, this schedule accepts that by having short soaks at intervals.  As glass is slow to absorb heat, it is necessary to use slow ramp rates and without pauses and changes in rates.  This should be applied all the way to the slumping temperature.

·        Holds of short durations are not effective at any stage in a slumping firing.  The objective is to allow the glass time to form to the mould with as little marking as possible.  This implies slow rates to low temperatures with significant holds at appropriate stages.  This about putting enough heat work into the glass that higher temperatures are not needed.

·        This kind of firing requires observation for new moulds and new arrangements of glass to ensure the slump is complete.  Once you know the mould requirements and are repeating the layup of the glass, the firing records will tell you what rates and times to use to get a complete slump with minimum marking.

·        The hold at annealing temperature is to equalise the temperature throughout the glass to produce a stress-free result.  Any soaks above are negated or repeated by the necessary soak at the annealing temperature.  The hold there must be long enough to complete the temperature equalisation that is the annealing.

·        My work has shown that annealing for one (3mm/0.125”) layer thicker produces a piece with less stress.  This indicates that a 6mm/0.25” piece should be annealed as for 9mm/0.35” to get the best result.

The summary of the firing strategy for slumping is:

• ·        A single ramp of a slow rate to the slumping temperature.
• ·        Observation of the progress of the slump to determine the lowest practical temperature and hold time.
• ·        Annealing for one layer thicker that being slumped.
• ·        Three stage cooling of the piece at rates related to the annealing hold.

Critique

This is a critique of the schedule. For comparison, my schedule for a full fused 6mm blank would be different.

• ·        140ºC/250ºF to 677º/1250ºF for 30 to 45 minutes.
• ·        9999 to 482ºC/900ºF for 1.5 hours
• ·        69ºC/124ºF to 427ºC/800ºF, no hold
• ·        125ºC/225ºF to 371ºC/700ºF, no hold
• ·        330ºC/600ºF to room temperature, off.

The rate of the published schedule is fast for a full fused blank and extremely fast for a tack fused blank. This needs to be slowed.  The schedule provides a single (fast) rate of heating, but with unnecessary holds.  The holds are so short as to be ineffective, anyway. There is no need for the holds on the way up to the slumping temperature.  In general slumping schedules are of fewer segments.   This is because glass behaves well with steady slow inputs of heat.

Then strangely, the schedule increases the rate to top temperature.  It does so with a brief soak at 593ºC/1100ºF.  This fast rate of 333ºC/ 600ºF begins at 400ºC/750ºF.  This is still in the brittle phase of the glass and risks breaking the glass.  The brittle stage ends around 540ºC/ 1005ºF.

This rapid rate softens the surface and edges of the glass without allowing time for the underside to catch up.  This explains uneven edges.  It also risks breaking the glass from too great expansion of the top before the bottom.

Additionally, the schedule uses a temperature more than 55ºC/100ºF above what is a reasonable highest slumping temperature.  The top temperature of this schedule is in the tack fusing range.

There is no need for a hold 55ºC/100ºF above annealing soak. It is the annealing soak that equalises the temperature before the cool begins.  The higher temperature equalisation is negated by the cooler soak at annealing temperature. So, the hold at the higher temperature and slow cool to the annealing temperature only delays the firing by about two hours.  It does not have any effect on the final piece.

The schedule is cooling for a piece of 12mm/0.5”.  This is slower than necessary.  As noted above, cooling for one layer thicker than the piece is advisable to get the most stress free result.  The annealing soak could be 1.5 hours following this idea.  Cooling with a three stage schedule reduces the risk of inducing temporary stresses that might break the glass.  Although the initial cooling rate I recommend is very similar to this schedule, it safely reduces the total cooling time.

• ·        69ºC/124ºF to 427ºC/800ºF, no hold
• ·        125ºC/225ºF to 371ºC/700ºF, no hold
• ·        330ºC/600ºF to room temperature, off.

Using my kind of schedule for the first time will require peeking once top temperature is reached to determine when the slump is complete. It may take as much as an hour. Be prepared to either extend the hold, or to skip to the next segment if complete earlier. The controller manual will explain how.

 More information is given in Low Temperature Kilnforming, An Evidence-based guide to scheduling.  Available from Etsy and Bullseye

Using Glass for Passivation in Semiconductor Applications

 

Robotic arm holding a silicon wafer for semiconductor processing. Image source: iStock.

A blog post by Krista Grayson of Mo-Sci rayson

In the fast-paced world of semiconductor manufacturing, where precision and reliability are paramount, choosing a suitable passivation material is critical to ensuring the optimal performance of electronic devices. Among the library of viable materials, glass has gained significant attention for its unique properties and versatility. This article looks at how glass is used for passivation and what properties make it highly suitable for the job.

Understanding Passivation in Semiconductors

Before unpacking the specifics of glass as a material for passivation, it is essential to understand the concept of passivation in semiconductor manufacturing. Passivation involves depositing a protective material onto the surface of metals or metal alloys to enhance their resistance to environmental factors.

The layering material can be organic or inorganic and should exhibit excellent electrical insulation and strong substrate adhesion, as well as block the ingress of chemical species. In the case of semiconductors, passivation is crucial to preventing degradation and ensuring long-term reliability.^1,2

Why Use Glass for Passivation?

Glass has emerged as a compelling choice for passivation due to its unique combination of properties. For example, glass can be formulated in numerous ways, with common types including Pb-Si-Al, Zn-B-Si, and Pb-Zn-B. This allows manufacturers to produce glass capable of meeting low and high-voltage electrical specifications; matching the coefficient of thermal expansion of semiconductor materials; and meeting the low temperature processing requirements.^3,4

Glass is chemically durable and thus can provide an inert barrier against external elements, such as moisture and contaminants, which might otherwise compromise the semiconductor’s performance. Moreover, the high transparency of some glasses, such as borosilicate glass, makes them ideal for applications with critical optical properties, such as photovoltaics. This transparency enables efficient energy transmission and absorption, contributing to the overall performance of semiconductor devices and solar cells.^5,6

How are Semiconductors Passivated?

Glass can be deposited onto semiconductors in a variety of ways. Choosing methods for passivation depends on factors such as the semiconductor device’s specific requirements, the passivation layer’s desired properties, and the overall manufacturing process. Methods for achieving glass passivation in semiconductor manufacturing include:⁷

• Chemical vapor deposition (CVD), including plasma-enhanced CVD (PECVD)
• Physical vapor deposition (PVD), including E-beam deposition
• Sputter Coating
• Atomic Layer Deposition (ALD)

In manufacturing, the process of glass passivation is frequently succeeded by chemical procedures, such as the etching of contact windows or the electrolytic deposition of contacts. These procedures may pose a threat to the integrity of the glass.

The chemical resistance of different passivation glasses varies significantly and serves as a crucial factor in determining the suitable glass type and the accompanying etching process.⁸

Comparing Glass to Other Materials

While various materials can be used for passivation, glass stands out for its exceptional stability over temperature, humidity, and time. Literature searches reveal a lack of head-to-head comparisons with other common passivation materials; however, general comparisons can be drawn.⁶

Amorphous silicon (a-Si) films utilized in solar cells present numerous advantages. These include a lower deposition temperature, in contrast to the temperatures commonly employed in cell manufacturing. However, it is essential to note that a-Si films exhibit sensitivity to subsequent high-temperature processes, which are frequently necessary in industrial manufacturing technology.⁹

Similarly, AlO_x passivation films can be applied at relatively low temperatures but can be limited by slow deposition speeds when using specific application methods. This can generate problems for high-throughput techniques, such as solar cell production.⁹

Polyimide, a common passivation material lauded for its strength and thermal stability, is also susceptible to moisture absorption. This can impact the strength and dielectric properties of the protective coating, risking the integrity of the semiconductor.¹⁰

Applications of Glass Passivation

Passivation glasses demonstrate outstanding performance in wafer passivation and encapsulation processes, providing advantages to a diverse range of semiconductor devices, including:⁸

• Thyristors
• Power transistors
• Diodes
• Rectifiers
• Varistors

Glass also has applications in solar cell passivation. In a recent study, researchers developed a method for enhancing borosilicate glass (BSG) passivation using high temperatures before lowering the temperature to accommodate the metallization process. In doing so, they notably improved the solar cell’s efficiency.¹¹

In another study, phosphosilicate glass (PSG) was found to significantly enhance the practical lifetime of minority carriers and improve the overall performance of solar cells, particularly in structures involving nanocrystalline silicon and crystalline silicon.¹²

Mo-Sci’s Expertise in Glass Thin Films

Fueled by the increasing prevalence of smart devices and advancements in the automotive and aerospace sectors, the semiconductor passivation glass market is anticipated to grow consistently in the next few years.³

Mo-Sci’s expertise lies in leveraging the unique properties of glass to create tailored solutions, ensuring the reliability and performance of many applications, including glass seals and glass coatings. Contact us for more information.

References and Further Reading

1. Pehkonen, S.O., et al. (2018). Chapter 2 – Self-Assembly Ultrathin Film Coatings for the Mitigation of Corrosion: General Considerations. Interface Science and Technology. doi.org/10.1016/B978-0-12-813584-6.00002-8
2. Lu, Q., et al. (2018). Chapter 5 – Polyimides for Electronic Applications. Advanced Polyimide Materials. doi.org/10.1016/B978-0-12-812640-0.00005-6
3. Reliable Business Insights. [Online] Semiconductor Passivation Glass Market – Global Outlook and Forecast 2023-2028. Available at: https://www.reliablebusinessinsights.com/purchase/1365249?utm_campaign=2&utm_medium=cp_9&utm_source=Linkedin&utm_content=ia&utm_term=semiconductor-passivation-glass&utm_id=free (Accessed on 05 January 2024).
4. Schott. [Online] Passivation Glass. Available at: https://www.schott.com/en-hr/products/passivation-glass-p1000287/technical-details (Accessed on 05 January 2024).
5. Zhong, C., et al. (2022). Properties and mechanism of amorphous lead aluminosilicate passivation layers used in semiconductor devices through molecular dynamic simulation. Ceramics International. doi.org/10.1016/j.ceramint.2022.07.191
6. Hansen, U., et al. (2009). Robust and Hermetic Borosilicate Glass Coatings by E-Beam Evaporation. Procedia Chemistry. doi.org/10.1016/j.proche.2009.07.019
7. Korvus Technology. [Online] The Revolution of PVD Systems in Thin Film Semiconductor Production. Available at: https://korvustech.com/thin-film-semiconductor/ (Accessed on 05 January 2024).
8. Schott. Technical Glasses: Physical and Technical Properties. Available at: https://www.schott.com/-/media/project/onex/shared/downloads/melting-and-hot-forming/390768-row-schott-technical-glasses-view-2020-04-14.pdf?rev=-1
9. Bonilla, R.S., et al. (2017). Dielectric surface passivation for silicon solar cells: A review. Physica Status Solidi. doi.org/10.1002/pssa.201700293
10. Babu, S.V., et al. (1993). Reliability of Multilayer Copper/Polyimide. Defense Technical Information Centre. Available at: https://apps.dtic.mil/sti/citations/ADA276228
11. Liao, B., et al. (2021). Unlocking the potential of boronsilicate glass passivation for industrial tunnel oxide passivated contact solar cells. Progress in Photovoltaics. doi.org/10.1002/pip.3519
12. Imamura, K., et al. (2018). Effective passivation for nanocrystalline Si layer/crystalline Si solar cells by use of phosphosilicate glass. Solar Energy. doi.org/10.1016/j.solener.2018.04.063

Refiring and Annealing

A question about re-fusing: 

I have just taken a large piece, with uneven layers out of the kiln, it went in … and fired for double thickness. A small piece has flipped and is 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, please. I will be taking it up to the lowest tack fuse temperature possible [my emphasis], 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. In this case, the major change is using a sinter firing – “the lowest tack fuse temperature possible”.

Ramp Up Rates

Previously the piece was in several layers.

• The piece is now a thicker single piece and needs more careful ramp rates.
• It is also of uneven thicknesses.
• And you intend to fire to a sharp tack or sinter.

These things make a requirement for more cautious firing. You cannot fire as quickly from cold as forthe 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 now could experience the differential expansion from  rapid heating, which can cause breaks. 

The previously fired piece will need a slower initial ramp rate this time. This is because you are firing for a sharp tack. This is also known as fusing to stick, or sintering. It is not because of a second firing. It is because of the differences in the glass for this firing. You are firing a single thicker piece of uneven layers to a sharp tack.

Looking at Stone* and the Bullseye chart for Annealing Thick Slabs indicates that in general, the first ramp rate should be halved for each doubling of calculated thickness. This is for full fused items. However, this is going to be a more difficult fusing profile - sintering. The calculation for sintering is as for 2.5 times the thickest part of the piece. This factor of 2.5 was determined by a series of experiments that are detailed in the eBook Low Temperature Kilnforming.

You started with firing two layers of 3mm/0.125” at possibly 330°C/595°F. You are now firing the fused 6mm/0.252 piece to a sharp tack. This means you should be looking at firing for 2.5 times or 15mm/0.625”. This implies 240°C/435°F as the maximum first ramp rate. A more cautious approach is to fire to 300ºC/540ºF at a rate of 72ºC/130ºF, as most heat-up breaks occur below that temperature. You should maintain that rate to 540°C/1005°F afterwards. 

Annealing

The annealing time and cool rate will be affected in the same way as the change to a sharp tack firing. Without that fuse profile change, and no change in the profile or thickness of the piece, it could have been annealed as previously. However, changing to a sharp tack means a longer anneal soak is required. This sharp tack annealing is for 2.5 times the thickness or 150 minutes.

Cooling

The cooling rates for this piece are not the same as for the first firing. A sharp tack firing will require cooling rates of:

• 40ºC/73ºF to 482°C/900°F.
• 72ºC/130ºF f427ºC/800ºF.
• 240ºC/435ºF to room temperature

This applies regardless of the fusing glass you are using, as it is the viscosity which is the important factor in cooling.  Viscosity is primarily related to temperature.

Refiring with Significant Additions.

Ramp rate

If there are additions to the thickness, a slower first ramp rate will necessary. If an additional 3mm layer is placed on top of a 6mm base for a rounded tack, you will need to schedule as for 19mm/0.75” (twice the thickest part). This will be 150°C/270°F for the first ramp rate. For a sharp tack, it will be as for 22.5mm/0.825”. The maximum rate will be reduced to 120ºC/216F for the first ramp. This shows the additional caution required for sharper fusing profiles.

Annealing

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 19mm/0.75”. This requires a hold of three hours at the annealing temperature and cooling over three stages:

• The first cool rate is 25°C/45°F per hour to 482°C/900°F.
• The second rate is 45°C/81°F per hour to 427ºC/800ºF.
• The last rate is at 90C°C/162°F per hour to room temperature.

If there are additions, plus firing to the lowest possible tack temperature – as in the example - the firing must be as for 2.5 times the actual thickness. Annealing as for 25mm/1” gives rates of:

• The first cool rate is 15°C/27°F per hour to 482°C/900°F.
• The second rate is 27°C/49°F per hour to 427ºC/800ºF.
• The last rate 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 re-fire a well-annealed piece without breaking it on the heat-up. It also shows that changing the profile to a sharper tack affects the annealing and cooling times and rates.

 

*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.

Go-to Schedules

 It’s a schedule I always use.

This is a frequent statement in response to a firing that has gone wrong.

You don't always fuse the same thing, or the same design, or the same thickness, etc. So why always use the same schedule?

The schedule for the firing each piece needs to be assessed individually. It may be similar to previous firings. But it may have differences. Assess what those differences mean for the firing.  Some factors to consider.

Addition of another layer to a stack in tack fusing makes a difference to the firing requirements. Even if it is only on part of the piece. It needs to have a slower ramp rate and a longer anneal soak and slower cooling.

A different design will make a difference in firing requirements too. For example, if you are adding a design to the edges of the glass, you will need different bubble squeeze schedules than when you do not have a border. It will need to be slower and longer than usual.

The placement of the piece in the kiln may require a re-think of the schedule too. If the piece is near the edge of the kiln shelf, or in a cool part of the kiln while others are more central, the same schedule is unlikely to work. You need to slow the schedule to account for the different heat work each piece will receive during the firing.

If you have introduced a strong contrast of colour or mixed transparent and opalescent glass in a different way, you may need slower heat ups and longer cools.

These are some examples of why the same schedule does not work all the time. It works for pieces that are the same. But it does not work for pieces that are different. And we should not expect it to.

There are sources to help in developing appropriate schedules. Bob Leatherbarrow’s book FiringSchedules for Kilnformed Glass is an excellent one.

Another one is especially good for lower temperature work: Low Temperature Kilnforming, anEvidence-Based Approach to Scheduling. Be aware that I have a vested interest here – I wrote it.

 

 

Differential Cooling of Transparent and Opalescent Glass

A statement was made on a Facebook group that transparent glass absorbs more heat than opalescent glass. And it releases more heat during cooling. The poster may have meant that the transparent heats more quickly than the opalescent, and cools more quickly.

Yes, dark transparent glass absorbs heat quicker than most opalescent (marginally), and it releases the heat more quickly (again marginally) than opalescent. The colour and degree of transparency do not absorb any more or less heat, given appropriate rates. They gain the same heat and temperature, although at slightly different rates due to differences in viscosity.

An occasional table

The rate of heating and cooling is important in maintaining an equal rate of absorption of heat. The temperature of both styles can become the same if appropriate lengths of heating, annealing, and cooling are used. The slightly different rates of heat gain can give a difference in viscosity and therefore expansion.  This slight mismatch during rapid ramp rates, might set up stresses great enough to break the glass. This can occur on the quick heat up of glass during the brittle phase (approximately up to 540ºC/1005ºF). In fact, most heat-up breaks occur below 300ºC/540ºF.

The main impact of differential heat gain/loss is during cooling. Annealing of sufficient length eliminates the problem of differential contraction through achieving and maintaining the Delta T = 5C or less (ΔT≤5C). It is during the cooling that the rates of heat loss may have an effect. The marginally quicker heat loss of many transparents over most  opalescent glass exhibits different viscosities and rates of contraction. The stresses created are temporary. But they might be great enough to cause breaks during the cooling. Slow cooling related to the thickness and nature of the glass takes care of the differential contraction rates by maintaining small temperature differentials.

Significance of Differential Heat Gain/Loss

Uneven thicknesses and the tack fusing profile both have much greater effects than the differential cooling rates of transparent and opalescent glass. It may be that strongly contrasting colours (such as purple and white) are also more important factors in heat gain and loss than transparent and opalescent combinations.  Cooling at an appropriate rate to room temperature for these factors will be sufficient to remove any risk of differential contraction between transparent and opalescent glasses.

Comparison of Citric Acid and Trisodium Citrate.

These two substances are useful means of removing kiln wash and refractory mould material from glass. They are important where abrasive methods such as sand blasting are not available or appropriate.

My recent experience with both citric acid and trisodium citrate shows differences in performance. This makes each more suitable in different contexts.

credit: Amazon

Trisodium citrate is the safest option when long soaks are required to remove refractory mould material. The trisodium citrate removes any risk of etching the glass on long soaks. It has been shown by Christopher Jeffree that two-day soaks in this will not etch the glass. It is most suitable for casting work.

Items cleaned with citric acid and vinegar
credit: Christopher Jeffree

Citric acid acts quickly on kiln wash, making long soaks less necessary. Depending on the thickness of the stuck kiln wash and the amount of agitation of the stuck kiln wash, the time required may be only a dozen minutes. It rarely takes more than a few hours.  Citric acid does not work quickly on refractory materials. This makes the trisodium citrate the better choice for long soaks.

 More on citric acid as a cleaner

 More on citric acid

More on trisodium citrate