A Sintering Project

Ready for firing

The project is to fire 6mm “balls” stacked 3 high onto a single sheet of clear glass without significant alteration to the base sheet or to the stacked balls. This creates a total thickness of 21mm. The proposal is to sinter the whole in one firing.

Scheduling for a sinter firing needs to be done as though 2.5 times the thickest part – in this case 52mm, or 2 inches

It is slightly more risky to do this in two firings, than one, in my opinion. A suggested schedule for sintering frit using Bullseye was:

• 100ºC /180ºF — 482ºC /900ºF, 60'  =5.8 hrs

• 40ºC /72ºF — 593ºC/1100ºF,10'      =2.8

• 20ºC /36ºF — 665ºC /1230ºF,30     =4.1

• Skip to anneal temperature, soak for 6 hours =6.5

• 6.7ºC /12ºF — 427ºC /800ºF,0'       =8.2

• 12ºC /22ºF — 371ºC /700ºF,0'        =4.7

• 40ºC /72ºF — room temperature,0’ =8.8

• Off                       =40.9 hours total or 1.7 days

This was annealing as for 38mm/1.5 inches thick. Annealing for 50mm/2” thick would need about 112 hours or 4.6 days.

However this schedule was not successful – the pieces were only lightly stuck together. Thinking about why, led to the proposal that the soak time and temperature were not long or high enough to give adhesion between the pieces.

A second attempt used a faster ramp rates to higher temperatures.

• 200°C /360°F – 540°C /1004ºF, 30’ =3.2 hrs

• 60°C /108°F -625°C /1157ºF, 30’     =1.92

• 30ºC /54ºF - 685ºC /1265ºF, 120’    =4.0

• skip to anneal temperature and soaked for 4 hours (as for 25mm/1”)

• 15ºC /27ºF – 427ºC /800ºF, 0’        =3.67

• 27ºC /49ºF – 370ºC /700ºF, 0’        =2.11

• 90ºC /162ºF – 50ºC /122ºF, 0’       =3.56

• Off

•  = a minimum total of 18.5 hours plus natural cooling of the kiln

This schedule used a:

• faster first ramp to a higher (540ºC /1004ºF) first soak

• a faster (60ºC /108ºF, which is 150% of the previous) rate to the lower slump temperature (625ºC /1157ºF)

• the same relative reduction (50%) in rate to a higher temperature (685ºC /1265ºF)

• a shorter (120’) anneal soak

• and consequently faster cooling rates, which showed no stress after firing

The whole structure held together and was sound. There was no apparent change in the size of the individual 6mm balls.

This difference in scheduling is an illustration of how time and temperature can be interchanged.

It also shows that size matters when sintering pieces together. Higher temperatures and more time are required for dots and balls than for frit.

More information is available in my e-book Low Temperature Kilnforming, available from Bullseye, Etsy and stephen.richard43@gmail.com

Time and Temperature

credit: timeanddate.com

Credit: Shutterstock

“What are the pros and cons on turning up the max temperature slightly Vs. a longer hold time”? Lea Madsen

This is a difficult question to answer, because there are variables such as

the temperature range,

the ramp rates, and soaks,

the forces acting upon the glass at a given temperature, 

the process,

the desired outcome of the firing,

etc. 

When talking about temperature vs. time, it is heat work that we are considering.  In many processes time and temperature are interchangeable, although the temperature range is important too.  This is a brief discussion of heat work in various processes.

Slumps

Slumping temperature is generally in the range of 620˚C-680˚C/1150˚F -1255˚F *, which is below the devitrification range.  This allows the exchange of time for temperature without risk, allowing more time rather than more temperature.  Higher temperatures cause more marking from the mould since the bottom of the glass is softer than at lower ones.  Lower temperatures give higher viscosity, so the glass is stiffer, resisting marks.

Low temperature fuses

Sharp tack fusing, freeze and fuse, some pate de verre processes, and sintering occur in the 650˚C -720˚C /1150˚F - 1320˚F range, risking devitrification only at the upper end of this range.  Extending the time rather than the temperature is important to maintain detail in these processes.  Higher temperatures will smooth the surface, risking loss of detail.  

Rounded tack processes (720˚C – 760˚C /1320˚F - 1400˚F)

These are within the devitrification range making the choice between time and temperature a balance of risks.  In my experience, it takes about an hour for visible devitrification to develop.  This means that you can extend the time, if the total time between the end of the bubble squeeze and the working temperature, including the hold time, is less than an hour.  It has the advantage of a more secure attachment between the pieces of glass, without altering the surface much. 

But if extending the soak time increases the time in the devitrification zone to be more than an hour, it is advisable to increase the temperature, rather than time.  Devitrification develops in the presence of air, so reducing the time in that range reduces the risk of devitrification developing.  The glass is moving during rapid ramp rates, reducing the chance of devitrification.

Drops

This includes drapes, and other free forming processes.  Kilnformers will be observing the progress of these firings, making it easier to balance temperature and time.  There are already long holds scheduled for the processes, so it is a matter of getting the right temperature.  If, after half an hour at the scheduled top temperature, the glass has not moved much, it is time to increase the temperature by, say 10˚C/18˚F and observe after another half hour, repeating the temperature increase if necessary.   Be aware of thinning the glass at the shoulder by setting a high temperature.  Free drops may take as much as 6 – 8 hours, so patience and observation are important to get good results.

Full fuse

At full fuse try to get the work done in 10 minutes to avoid complications with devitrification.  So, increasing the temperature rather than the length of the soak seems best.

Flows

Whether frit stretching, making pattern bars, pressing, etc., low viscosity is important.  Viscosity is closely related to temperature, so increasing the temperature is the better choice.  Increasing time without increasing temperature does not change viscosity much.

Casting

Extending time at top temperature seems best for open face casting, as the temperature is already high.  A slow ramp rate to that top temperature may make adding time unnecessary, because the heat work will be increased by the slow rise.  Experience has shown that a rate of 200˚C/360˚F is enough to avoid devitrification.  With enclosed castings devitrification is not such a risk, so time can be added without concern.

 

Observation

In all these processes it is advisable to observe the progress of the firing by quick peeks to determine the effective combination of temperature and time.  Also note that heat work is cumulative, making for changes in profile with repeated firings. 

 

* The softening point of float glass is around 720°C/1328°F, so the slumping range is about 700°C/1292° to 750°C/1382°F.

Sample Tiles

credit: Tia Murphy

There are advocates for making tiles as references for future work.  

• They show the profiles achieved at different temperatures.  
• They can be stored for easy visual reference when planning a firing.  
• It is a useful practice for any kiln new to the user.  

These tiles are assembled in identical ways to enable comparisons.  They should include black and white, iridised pieces- up and down, transparent and opal, and optionally stringers, confetti, millefiori, frit and enamels.  

The tiles are fired at different top temperatures with the same heat up schedule with the top temperature of each at about 10C or 20F intervals.  These show what effect different temperatures give.  Start the temperature intervals at about 720C or 1330F.

This is a good practice, even if time consuming.  It gets you familiar with your kiln and its operation.  It gives a reference for the profiles that are achieved with different temperatures at the rates used.

Ramp rate and time

But, as with many things in kilnforming, it is a little more complicated.  The effect you achieve is affected by rate and time used as well as the temperature.

The firing rate is almost as important as the temperature.  

• A slow rate to the same top temperature will give a different result than a fast rate.  
• The amount of heat work put into the glass will affect the temperature required.  
• Slow rates increase the time available for the glass to absorb the heat.  
• Glass absorbs heat slowly, so the longer the time used by slower rates, the rounder the profile will be.

Since time is a significant factor in achieving a given profile, any soaks/holds in the schedule will affect the profile at a set temperature.  A schedule without a bubble squeeze will give a different result than one with a bubble squeeze at the same temperature.

To help achieve knowledge of the rate/time effect, make some further test tiles.  Use different rates and soaks for the test tiles of the same nature as the first temperature tests. But vary only one of those factors at a time. Consider the results of these tests when writing the schedule for more complex or thicker layups. 

Mass

Also be aware that more mass takes longer to achieve the same profile.  Slower rates and longer times will help to achieve the desired profile at a lower temperature.  It is probably not practical to make a whole series of test tiles for thicker items.  But, a sample or two of different thicknesses and mass will be helpful to give a guide to the amount of adjustment required to achieve the desired outcome.

The results of sample tiles are due to more than just temperature.  They are a combination of rate, time, and temperature (and sometimes mass).  These factors need to be considered when devising or evaluating a schedule, because without considering those factors, it is not possible to accurately evaluate the relevance of a suggested top temperature.

See also: Low Temperature Kilnforming, available from Bullseye and Etsy

Kilnforming with 3mm Glass

 A power point presentation I made a few months ago to the group Lunch with a Glass Artist.

It is 33 slides long.

Kilnforming with 3mm Glass.pptx