Monday, 4 July 2016

Slump Point Test

At a time when we are all going to be trying a variety of glass of unknown compositions to reduce costs of kiln working, the knowledge of how to determine the slump point temperature (normally called the softening point in the glass manufacturing circles) and the approximate annealing temperature becomes more important.  This is called the slump point test.

This test can be used to determine both the slumping point and the annealing soak temperature. This used to be required when the manufacturers did not publish the information. It continues to be useful for untested glasses.

The method requires the suspension at a defined height of a strip of glass, the inclusion of an annealing test, and the interruption of the schedule to enter the calculated annealing soak temperature.

A strip of 3 mm transparent glass is required. This does not mean that it has to be clear, but remember that dark glass absorbs heat differently from clear or lightly tinted glass. The strip should be 305 mm x 25 mm.  If you are testing bottles, you may find it more difficult to get such a long strip.  My suggestion is that you cut a bottle on a tile saw to give you a 25 mm strip through the length of the bottle.  Do not worry about the curves, extra thickness, etc.  Put the strip in the kiln and take it to about 740C to flatten it. Reduce the temperature to about 520C to soak there for 20 minutes.  Then turn the kiln off.  

Suspend the strip 25 mm above the shelf, leaving a span of 275 mm. This can be done with kiln brick cut to size, kiln furniture, or a stack of fibre paper.   Make sure you coat any kiln furniture with kiln wash to keep the glass from sticking.

The 305mm strip suspended 25mm above the shelf with kiln furniture.

Place some kiln furniture on top of the glass where it is suspended to keep the strip from sliding off the support at each end. Place a piece of wire under the centre of this span to make observation of the point that the glass touches down to the shelf easier.

The strip held down by placing kiln furniture on top of the glass, anchoring it in place while the glass slumps.

Also add a two layer stack of the transparent glass near the suspended strip of glass to act as a check on whether the annealing soak temperature is correct. This stack should be of two pieces about 100 mm square. If you are testing bottles, a flattened base or neck will provide about the same thickness.  This process provides a check on the annealing temperature you choose to use.  If the calculated temperature is correct there should be little if any stress showing in the fired piece.

The completed test set up with an annealing test and wire set at the midpoint of the suspended glass to help with determining when the glass touches down.

The schedule will need to be a bit of guess work.  The reasons for the suggested temperatures are given after this sample initial schedule which will need to be modified during the firing.

Ramp 1: 200C per hour to 500C, no soak
Ramp 2: 50C per hour to 720C, no soak
Ramp 3: 300C per hour to 815C or 835C, 10 minute soak
Ramp 4: 9999 to 520C, 30 minute soak
Ramp 5: 80C per hour to 370C, no soak
Ramp 6: off.

Fire at a moderate rate initially – 200C/hr to 500C - and then at 50C/hr until the strip touches down. This is to be able to accurately record the touch down temperature.  If you fire quickly, the glass temperature will be much less than the air temperature that the pyrometer measures.  Firing slowly allows the glass to be nearly the same temperature as the air.  

Observe the progress of the firing frequently from 500C onward, unless it is float glass you are testing. Then you can start observing from about 580C. Record the temperature in Celsius when the middle of the glass strip touches the shelf. The wire at the centre of the span will help you determine when the glass touches down.  This touch down temperature is the slump point of your glass.  You now know the temperature to use for gentle slumps with a half hour soak.  More angular slumps will require a higher temperature or much more time.

Once you have recorded the slump point temperature, you can skip to the next ramp (the fast ramp 3).  This is to proceed to a full fuse for soda lime glasses. Going beyond tack fusing temperatures is advisable, as tack fuses are much more difficult to anneal and so may give an inaccurate assessment of the annealing. Most glasses, except float, bottles and borosillicate will be nearly fully fused by 815C. If it is float, bottles or borosilicate that you are testing, try 835C. If it is a lead bearing glass, lower temperatures than the soda lime glass should be used. In all these cases observation at the top temperature will tell you if you have reached the full fuse temperature. If not add more time or more heat to get the degree of fuse desired.

While the kiln is heating toward the top temperature you can do the arithmetic to determine the annealing point.  To do this, subtract 40C from the recorded touch down temperature to obtain an approximate annealing point.  This is approximate as the touch down temperature is by the nature of the observation also approximate.  For example, the touch down temperature might be 600C

The next operation is to set this as the annealing soak temperature in the controller. This will be the point at which it may be possible to interrupt the schedule and change the temperature for the annealing soak that you guessed at previously. Often though, you need to turn the controller off and reset the new program.  Most times the numbers from the last firing are retained, so that all you need to do is to change the annealing soak temperature.

The annealing soak should be for 30 minutes to ensure an adequate anneal. This may be excessive for 3 mm glass, but as the anneal test is for 6 mm, the longer soak is advisable. The annealing cool should be 80C/hr down to 370C. This is a moderate rate which will help to ensure the annealing is done properly. The kiln can be turned off at that temperature, as the cooling of the kiln will be slow enough to avoid any thermal shock to the annealing test piece.

When cooled, check the stack for stress. This is done by using two polarised light filters. See here for the method. 

squares of glass showing different levels of stress from virtually none to severe
 (no light emanating to strong light from the corners)

If the anneal test piece is stressed there is a problem. There could be a number of reasons for the inadequate annealing. It could be that the glass has devitrified so much that it is not possible to fuse this glass at all. If you also test the suspended strip for stresses and there is very little or none, it is evidence that you can kiln form single layers of this glass. You now know the slumping temperature and a suitable annealing temperature and soak for it, even though fusing this glass is not going to be successful.

Other reasons for stress due to inadequate annealing could be that the observations or calculations were incorrect.  

  • Of course, before doing any other work, you should check your arithmetic to ensure the calculations have been done correctly. I'm sure you did, but it is necessary to check.  If they are not accurate, all the following work to discover the difficulties will be fruitless.
  • The observation of the touch down of the suspended strip can vary by quite a bit - maybe up to 15C. To check this, you can put other annealing test pieces in the kiln.  This will require multiple firings using temperatures in a range from 10C above to 10C below your calculated annealing soak temperature to find an appropriate annealing soak temperature.
  • If stress is still showing in the test pieces after all these tests, you can conduct a slump point test on a strip of glass for which there are known properties. This will show you the look of the glass that has just reached touch down point as you know it will happen at 40 C above the published annealing point.  You can then apply this experience to a new observation of the test glass. 

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