The Importance of Viscosity in Slumping

 What is viscosity?

The official definition is that it is a measure of the resistance to flow, e.g., honey vs water, or hard vs soft glass.  Honey and hard glass have greater resistance to flow. 

Importance of viscosity

In slumping, large differences in viscosity of the combined glasses will have different rates of deformation across the piece.  There is the possibility of uneven slumps as a result.  The stresses between the different viscosities may cause breaks or splits with rapid temperature rises.  Combining large differences in viscosity requires more caution in ramp rates and in annealing and cooling.  Of course, unusual results can be obtained by manipulating time and temperature.

Effect of temperature

Viscosity is affected more directly by temperature than heat and time.

Credit: Bullseye Glass Company

There are frequent statements about viscosity such as dark glass is less viscous than light, or transparent is less viscous than opalescent.  Also, Bob Leatherbarrow ran some slumping testes showing thick glass slumped less at a given temperature than thin.  Further, Ted Sawyer mentioned to me that some opalescent is less viscous than some transparent glass.   My experience is different, so I wanted to test my assumptions against theirs.

Experiment setup

25mm/1" wide strips were suspended with a span of 20cm/8".  Weights were placed on ends to avoid any slipping.  

Does comparative viscosity vary with temperature?

I fired samples at three temperatures and times

• 600C for 30 minutes
• 650C for 1 minute
• 690 for 1 minute

All at 150C/hr to top temperature.  The short soak time for the higher temperatures were because the glass deformed so quickly.

Results

Bullseye glass. Span of 20cm. Fired at 150C/hr to 600C for 30 minutes

            Code - name - deformation from horizontal

0126 Light Cyan              16mm

0243 Translucent White    20mm

0013 Opaque white         21mm

1101 Clear Tekta             21mm

0100 Black                     24mm

0141 Dark Forrest Green 24mm

1122 Red                       24mm

0161 Robbins egg blue    26mm

0137 French vanilla        27mm

1427 Light amber           27mm

1428 Light violet            29mm

0303 Dusky lilac            32mm

1125 Orange                 32mm

0147 Deep cobalt blue   33mm

0113 White  (.0038)      34mm

0126 Orange                 35mm

1246 Copper blue          37mm

1320 Marigold yellow     40mm

1341 Ruby pink sapphire 40mm  

(special production)

Most opals in this test were more viscous than the transparent glasses.  There are some exceptions such as Dusky lilac, Cobalt blue, Orange.  There were some exceptions too in the transparents: black, red, light amber.

Bullseye glass. Span of 20cm. Fired at 150C/hr to 650C for 1 minute

            Code - name - deformation from horizontal

0100 Black                    26mm

0013 Opaque white        30mm

1122 Red                      30mm

1428 Light violet           30mm

0243 Translucent white  31mm

0141 Dark forest green 31mm

0161 Robins egg blue    31mm

0147 Deep cobalt blue   32mm

0126 Orange opal          32mm

1101 Clear tekta           33mm

1125 Orange                34mm

0137 French vanilla       35mm

0216 Light Cyan            38mm

0303 Dusty lilac            38mm

1341 Ruby pink sapphire 39mm

1437 Light amber          41mm

1320 Marigold yellow     41mm

1246 Copper blue          43mm

0113 White  (.0038)      45mm

Some odd results appeared in this firing.  Black deformed least and white most. But in general, the opal was again more viscous than the transparent.  Exceptions were the red, and light violet in the transparents; and among the opalescents were the light cyan, dusty lilac and white.

Also of note is that the amount of deformation was very similar for the test at 600C for 30 minutes and the one at 650C for only 1 minute.  This re-inforces the concept that time and temperature are often interchangeable, so longer at a low temperature can equal the heat work effects of a shorter soak at a higher temperature.

Bullseye glass. Span of 20cm. Fired at 150C/hr to 690C for 1 minute

            Code - name - deformation from horizontal

0013 Opaque white        35mm

0141 Dark forest green   41mm

0137 French vanilla        44mm

1101 Clear                    49mm

1428 Light violet            52mm

0126 Orange                 53mm

0303 Dusty Lilac            54mm

1437 Light amber          54mm

0113 White   (.0038)     54mm

0243 Translucent white  55mm

1125 Orange                 56mm

1341 Ruby pink sapphire 59mm

1122 Red                      59mm

0161 Robins egg blue     60mm

0147 Deep Cobalt blue   62mm

1320 Marigold yellow     67mm

1246 Copper blue          90mm

The results of the higher temperature in this test showed variations in comparative viscosity.  Some opals (e.g., dark cobalt blue, robins egg blue) were less viscous than most transparents, but some transparents (e.g., light violet and light amber) were more viscous than most opals.

The test shows wide variability in the viscosity of transparent colours at a higher temperature.  It appears that hot and deep colours are the least viscous of the transparent colours in this test.  There are also significant differences in the viscosity of opalescent and transparent glasses of the same colour.  It is apparent that not all glasses have the same rate of viscosity change with the same rate of temperature change.

Summary

This test showed that in general, the opals in the test are stiffer than the transparent from 600C to 690C with some exceptions.  It appears transparent hot colours are less viscous than the light transparent colours.  This is not the same for opalescent colours which seem to have a wider range of viscosity at these temperatures.

The similar deformation of the test glasses at 600C for 30 minutes and at 650C for one minute, shows the possibility of using lower temperatures and longer times to achieve the same effects in slumping as at higher temperatures with shorter soaks.

Viscosity and expansion rate are roughly related at lower temperatures, but both change rapidly above the softening point.  This experiment demonstrates that expansion rates vary within a single fusing compatible range of glass.  Also, glass with significantly different viscosities can be compatible, since this was all Bullseye fusing compatible glass.

It is apparent from this unscientific experiment that when preparing for slumping an important piece that combines different colours and styles, testing for relative viscosity is a good idea to determine if there are widely different viscosities.  This knowledge will enable an accommodation to be made in scheduling.

Tom Sawyer comments on the subject of viscosity:

“Viscosity is not always lower for transparent glasses than for opalescent glasses.  Opalescent glasses will begin to move more at temperatures of 538ºC/1000ºF than will transparent glasses, and even at 677ºC/1250ºF, there are still some opalescent glasses that move more than many transparent glasses.  It is only when we get to fusing temperatures that we begin to see the majority of transparent glasses moving more than the majority of opalescent glasses.  In general, it is correct that darker glasses will move more than lighter glasses – both because of their chemistries and because of their greater propensity to absorb infrared energy.”

More information on the effects of viscosity in kilnforming can be found in the ebook Low Temperature Kilnforming.

Deep Slumps with Bubbles

 

Photo Credit: Rachel Meadows-Ibrahim

The main causes of the large thin bubble is most probably  too high a temperature combined with a long soak.

Elevation of the Mould

The poster indicated there are eight holes total – four on the sides and four under the glass. This means any air has an exit out from under the glass and from the inside of the mould. So, in this case it does not need to be elevated for exit of air.  In my practice l have never, except in tests, elevated my slumping moulds. I have not had failures. My experiments involved in writing the eBook Low Temperature Kilnforming  showed no significant temperature differences between elevating, or not, below the mould.

Effect of Fast Rates

Slow rates to low temperatures with long soaks avoid sealing the glass to the mould. This means air can move out from under the glass during the slump. 

• Fast rates, and elevated temperatures can restrict air movement from under the slumping glass.  
• Fast rates and high slump temperatures can each cause uprisings because the glass slides down the mould during the soak, and that weight pushes the bottom upwards.

Temperature and Uprisings

This uprising is different from the bubble at the bottom on this piece. It is possible to see the glass bubble is thinner than the surrounding glass. As there were holes for air to escape, it seems the temperature and or speed was great enough to allow the glass to form to the mould at the bottom.  This covered the air holes and allowed the remaining air to push upwards on the glass.  A lower top temperature may have avoided this bubble formation.  Certainly, a combination of a slower rate and a lower temperature would have avoided the formation of the bubble.

Observation

Further, observation during the firing would have caught this bubble formation early enough to skip to the annealing and result in a piece with only a slight uprising, and before it became a bubble. Peeking should start at the beginning of the slumping soak and be repeated at 5 to 10 minute intervals.

Visible Devitrification

"Why does devitrification appear on slumped pieces?"

A brief explanation 

Scientific research in developing a glass matrix to support bone grafts gives some information.  This kind of glass matrix requires to be strong.  Development showed that devitrification weakens the matrix.  The crystals in a matrix are not as strong as the amorphous glassy state.  So, devitrification needs to be avoided.

The research to avoid devitrification showed that it begins at about 600˚C/1110˚F.  It only begins to become visible above 700˚C/1300˚F.  The process developed was to introduce a “foaming” agent.  The process fired slowly to 600˚C/1110 ˚F and then quickly to 830˚C/ 1530˚F.  It left a strong open matrix around which bone can grow. Although the research used float glass, it is also a soda lime glass, just as fusing glasses are.  The formation of devitrification begins at the same temperature for fusing glasses as for float.

The result of this medical research shows that devitrification begins on glass before it is visible. Devitrification is cumulative. A little becomes greater with another firing.  This is so even with good cleaning between firings. The new devitrification builds on the previous.  It does this from 600˚C/1110 ˚F.

A subsequent firing can continue this devitrification to the point where it is visible. This can happen, although the temperature at which we can see it after one firing has not been reached.  This continued devitrification at low temperatures can become great enough to be visible at the end of one or multiple slumps.

Credit: Bullseye Glass Co.

What can we do?

Clean all the glass before every firing very well.

·         Avoid mineralised water.

·         Final clean with isopropyl alcohol.

·         Polish dry at each stage with white absorbent paper.

 

Soak longer at lower temperatures.

·         Use longer soaks to achieve the slump.

·         Keep the temperature low.

·         Observe the progress of the firing with quick peeks.

 

Use slower ramp rates.

·         Slower rates enable the heat to permeate the glass.

·         Enables a lower slump temperature.

 

If there is any hint of devitrification after the first firing,

·      use a devitrification spray, or

·      provide a new surface.

• o   remove the surface by abrasion on sandblasting,
• o   cap with clear, or
• o   cover whole surface with a thin layer of clear powder.

·      Fire to contour fuse to give a new smooth surface.

·      Clean very well and proceed to slump.

Changing size in Slumping

 “I have full fused a single piece of glass with a few small pieces on top.  I thought it would shrink some as I had been told, but it maintained its size and still fit the mold for slumping.” 

I believe the enquirer is talking about a single layer circle changing size at full fuse.  Dog boning is much less evident in circles than rectangles.  The glass retreats evenly all along the edge.  This gives the appearance of retreating less than rectangles.  The absence of any big change in size may also result from thinning of the centre.  The amount of size change will be affected by the temperature of the full fuse too.  In this case there were additions which will have resisted any tendency to shrink.

Lower top temperatures, more rapid ramp rates to the top, and shorter holds will have the effect of limiting the movement of glass toward 6mm thick.

credit: Bullseye Glass Co

The viscosity of glass at full fuse is enough for it to attempt to pull up to 6mm. At casting temperatures, the viscosity is so low that 6mm of glass spreads out.  Temperature affects viscosity.

 

At slumping temperatures (620˚C - 680˚C / ca.1150˚F - 1260˚F), the viscosity high enough that the dimensions of a circle do not change. A circular piece of 3mm glass held at slumping temperatures does not change dimension.  It may, if held long enough take on a kind of satin sheen, rather than a fire polish.  But the viscosity  is low enough to allow the glass to form to the mould, given sufficient time. The resulting slumped piece will appear to be smaller than the mould. If you measure the piece around its outside curve, you will find the distance is almost the same as the diameter of the blank. 

 

Changing size on a single layer piece is dependent on the temperature and heat work applied to the piece.

Bowl Split Analysis

The visual evidence relating to this enquiry is a sharp-edged break through the middle of the slumped piece. The two parts have slumped separately, and seem attached at the rim, leaving the middle opened.  A moderate slumping temperature was used to fire the piece at the bottom of a stacked kiln load.

This is used as an example of the kind of thinking required when investigating breaks in slumping.

The split occurred before the slump was complete. We know this because the pieces no longer fit exactly together.  This means the crack opened as the slump continued.  There is other evidence.

The opening of the crack cannot have happened at or after the annealing. It would have already formed to the mould in a whole state. It would break completely across, because it would be in a brittle state.  And the pieces would fit exactly together.  But they do not.

This piece was at the bottom of a stack of shelves in a deep kiln.  At the bottom, there is no radiant heat, only side heat.  This could be a major cause the kind of break described.

It is possible that the split was not across the whole piece.  At the bottom of the kiln, the glass is not receiving any radiant heat from the top.  It is getting radiant heat only from the sides of the kiln.  That means the edges were considerably hotter than the centre.  The edge may be in a plastic state while the centre is still in the brittle state.  The contrasts in expansions are often great enough to break a piece.

From the evidence we have, it can only be said the ramp rate was too fast for the conditions. 

This little exercise shows that a lot of information about layup, schedule, place in the kiln, and any other relevant variation on the usual, must be detailed when asking why something has not turned out as expected. 

 

 

Slumping Breaks on “go-to” Schedules

 An "It has always worked for me before" schedule implies a single approach to slumping regardless of differing conditions.  Layup alterations, thickness variations, colour contrasts, mould variations all affect the scheduling.  The schedule for each piece needs to be altered when there are changes from the schedule for the “standard” piece, or mould.

Photo credit: Emma Lee

In the example shown, we are not told the schedule, but it shows that the rate was a little too fast. If it had been faster the glass would have separated further apart. The heat was enough to appear to recombine at the edges where it was not slumping so much. 

Review your "go to" schedules whenever something changes. It may still be a good base from which to work. But you need to assess the layup, thickness, and any other variations to help adjust the schedule to fire each piece.

Some of the variations from the “standard” to be considered are:

Single layer slumping 

Weight

Mould sizes

Relative Slumping Depth

Mould shape and detail

Diagnosing Slump fractures

Once you have an initial idea of the source of the problem, think about it.  Test it against the evidence.  Is there enough evidence to make a call?  Make sure you have considered alternative explanations.  It is just too easy to make a snap decision about causes in low temperature processes.  The source of breaks in slumping are most often complex and stem from interrelated factors.

I give you an example of the difficulties of diagnosing a slumping break.

On a Facebook group a person showed the break of a single layer on a cyclone mould.  Others commented the same had happened to them.

Picture credit: Esther Mulvihill Pickens

Possible causes suggested on Facebook included:

• Thermal shock on the way up
• Thermal shock on the way down
• Too large on the mould and broke due to differential contraction
• Too many holds on the way up
• Too hot
• Too thin
• Follow the CPI programme
• Glass extending over the sides

Some of these suggestions were of general applicability, some in relation to the state of the broken glass.

The suggestions did not include:

• Cause of the rounded dots at the bottom of the mould.
• A cause for the state of the flat piece off the mould (it appears sharp edged.  Does it show some forming already?).
• The cause for the location of the fully formed remaining glass.
• The effect of the location of the mould and glass in the kiln.
• The consequences of a short soak at top temperature. 
• Is the kiln running hotter than most (1290ºF/698ºC for 10 minutes at top temperature was used)?

Of course, it is difficult to diagnose a problem from just one picture. It is difficult even with many pictures. And so, without handling the object, only suggestions can be made.

But….

You must spend enough time examining the piece with whatever other information is available to make specific suggestions.  The first thought may not consider all the factors.  Consider what kinds of causes there are for breaks during or after slumping.

More close inspection reveals the rounded edges of the break.  That supports the idea that the temperature was too high. It also supports the diagnosis that the break occurred on the heat up.

The edges of the piece that has fallen off the mould, and now rests on the shelf, seem to be square or sharp. This shows the extent of the difference of temperature between shelf and top of the mould – less than 100mm/4 inches.  Also, how small the differences in temperature are between slump and tack.  The extent of difference in fusing does depend on how high in the kiln the mould is placed.  That is demonstrated here by the different elevation of the two pieces. 

The conformation of the glass to the mould is complete.  This supports the diagnosis of the break occurring early in the firing, and certainly before the slump was complete.  These pieces will not fit together.  So, even if the edges were sharp the fact they will not fit together shows they conformed independently to the mould surface.  Therefore, the break was before forming temperature was reached.

The glass hangs over the mould edges on only three sides and at an angle.  This indicates the cause of the overhang was the break.  Not the reverse. An overhang at the beginning of the slump is likely to be even.

The piece on the floor of the kiln combined with the movement of the glass toward the back gives an indication that the origin of the break is at the front.  This relates to uneven temperatures and to the placement of the mould.

No one mentioned the placement of the mould and glass at the back of the kiln.  This will have an effect on scheduling.  The mould and glass are very large in relation to the kiln.  There is little space between the glass on the mould and the walls of the kiln.  Also, the mould is placed asymmetrically in the kiln – very close on three sides.  This will cause uneven heating in any kiln.  To have a successful firing of glass on this mould in this kiln will require radically different schedules to that for a centrally placed mould that is moderate for the size of the kiln.

The large size (relative to the kiln) and the asymmetrical placing are the causes of the break, in my opinion.  I admit that it took me several looks to realise the placement was a key cause of the break.

So, the generalised comments about thermal shock are correct, but not as to the cause of that shock.  The kiln will be hotter in the central part and cooler at the corners.  This is true of all rectangular kilns.  The important thing is to learn how to cope with these temperature differences.

Slow firings to low temperatures with long soaks are the three important elements.  These make up the heat work of the kiln. Applying this to a schedule means:

• slow ramp up rates – as little as one half the recommended rates for centrally placed moulds that are moderately sized in relation to the kiln.
• Low temperatures present lesser risks to the control of the outcome of the firing.  Determining the lower temperature possible requires peeking into the kiln to monitor the progress of the firing.
• Long soaks combined with low temperatures get the kilnforming done with minimal marking of the underside.  Low temperature soaks - in excess of 30 minutes - are required to minimise the marking.  Observation of the slump will be necessary to determine when it is complete.

My suggestions for the causes of other elements are:

·        Cause of the rounded dots at the bottom of the mould.

The temperature was too high. 698ºC/1290ºF is much hotter than needed for a slump. It was hot enough to round edges and small shards of glass.  Which shows excessive heat was received by the glass.

·        A cause for the state of the flat piece off the mould (it appears sharp edged. Does it show some forming already?)

The soak of 10 minutes was too short for the temperature in the kiln to equalise from top to bottom.  The glass on the shelf may not have reached 650ºC/1200ºF with such a short soak.

·        The cause for the location of the fully formed remaining glass.

The glass broke and was forced apart by the size of the expansion differences within the glass.  The movement of a piece at the front of the mould combined with the rearward and side movement of the glass indicate the origin of the break was at the front.  The distance apart shows the amount of force, and so the degree of reduction in the ramp rate required to fire this successfully.

·        The effect of the location of the mould and glass in the back of the kiln has already been discussed.

·         The consequences of a short soak at top temperature.

A high temperature is often considered necessary to pick up all the detail in moulds, whether slump or texture moulds.  The same effect can be achieved at lower temperatures with longer soaks.  The results of this strategy are fewer mould marks on the bottom of the work.

·        Is the kiln running hotter than most (Used 1290F/698C for 10 minutes at top temperature)?

This is one that cannot be answered other than by experiments carried out by the owner of the kiln.  Look at the Bullseye Tech Note #1 Knowing your Kiln for methods of testing temperatures. 

In short:

Diagnosis of slumping breaks is more complex than it appears at first.

More information is available in the eBook Low Temperature Kilnforming, an Evidence Based Approach to Scheduling.

This is available from Bullseye or Etsy

Slumping and Annealing bottles

"Can a tack fuse schedule for fusing glass can be used to slump bottles?"

It may be that this person does not have the confidence to write a new schedule.  They may wish to use an existing schedule for another purpose. The short answer is “Although a Bullseye or Oceanside tack fuse temperature will be high enough to slump bottles, they are not suitable for annealing”.  There are reasons for this. 

The softening point of float glass, which is similar to bottle glass, is 720ºC/1330ºF.  Slumping would normally be done at about 20ºC/36ºF above this. You also need a slumping hold at this temperature much longer than a tack fuse schedule would use.

if you use a tack fuse schedule for a fusing glass, your annealing will be inadequate. Bottle and float glass tend to have an annealing point of around 540ºC/1005ºF. An annealing for fusing glass will be between 515ºC/960ºF and 482ºC/900ºF.  This is likely to be too low an annealing point for bottles.  Also, the annealing soak is likely to be too short. Slumped bottles are very thick at the base where it folds over the cylinder of the bottle.  This requires a longer anneal soak and slower cool than a schedule for a tack fuse of fusing glass.

Checking for stress in the completed work is normal.  It is essential for your finished bottle if you use a tack fuse to fire it.

 

Schedules should be devised for the glass and layup of each piece. Transferring a schedule for fusing to bottle glass is unlikely to be successful.

Slumping contrasting colours and styles

 A question about why a tack fused 6mm/0.25” piece of combined dense white and black in a slump firing broke has been raised.  Other pieces of black and other whites also tack fused in the same firing did not break.

"Living in the Grey" Stephen Richard

Contrasting colours

Combining the most viscous and the least viscous of bullseye glasses - dense white and black - is a challenge.  The survival of other pieces in the firing with slightly less viscous white give an indication.  Their survival shows that the anneal and cooling conditions were too short and fast for the broken piece. 

It may be worth checking how much stress is in the surviving pieces.  It may not be possible directly on these fired pieces. There is a way.  Mock up the black and white in the same way as the surviving pieces.  Put this on a larger clear piece and fire in the normal way. This enables you to see stress in opalescent layups. If there is any, it is revealed on the clear by using polarising filters. 

The usual recommendation is to anneal and cool as for twice the thickness was followed in this firing.  It is important to anneal and cool more conservatively in cases of contrasting colours. Strongly contrasting colours and styles (low viscosity transparent and high viscosity white opalescent) require more time at annealing and need slower cooling.  I do that by using a schedule for one layer thicker than calculated.  In this case, as for 15mm/0.61” (two tack layers needs firing as for four tack layers, plus one extra for the high and low viscosity combination).

Viscosity

The reasons for this are viscosity:  

·        Annealing is done at a temperature that achieves a viscosity of around 10^13.4 poise. It can be done in a range from there toward the strain point of 10^14.5 poise.  Below the strain point temperature (which is determined by the viscosity), no annealing can occur.  The glass is too stiff.  The closer to the strain point that the annealing is done, the more time is required at the annealing temperature.

·        The annealing of Bullseye is already being done in the lower range of viscosities. It is possible the viscosity of the white is so high as to be difficult to anneal with the usual length of soak.

·        Although I do not know the exact viscosities of dense white and soft black at the annealing temperature, it is known white has a higher viscosity than the black.  The means to achieve less stress in the glass is to hold at the annealing temperature longer than normal.  A cooling schedule related to the length of the anneal hold is needed.  This information can be obtained from the Bullseye chart for annealing thick glass.  The rates and times apply to all soda lime glass, which is what fusing glass is. Only the temperatures need to be changed to suit the characteristics of your glass.

Slumping

The slumping of this combination of high and low viscosity glasses requires more care too.  My research has shown that the most stress-free result in slumping is achieved by firing as for one layer thicker than that used for the fuse firing.  For a tack fuse, this means firing for twice the thickness, plus one more layer for contrasting colour and style.  Then schedule the slump by adding another layer to the thickness.  This means scheduling as for 19mm/0.75"instead of as for 12mm/0.5”.  This is to account for profile, contrasting colours, and stress from slumping.  This is about three times the actual height of the piece.  

Slumping tack fused pieces of contrasting colours requires very cautious firing schedules.  These longer schedules need to have a justification.  It is not enough to add more time or slow the cooling just in case.  Excessively long anneal soaks, and slow cools can create another set of problems. 

More viscous glass needs more time at the annealing soak to an even distribution of temperature between the more and less viscous glasses.

More information about other low temperature processes can be found in my eBook Low Temperature Kilnforming.  Available from Bullseye and Etsy