Glaze & Clay Tutorial - 10

[Editor's note: print this document with a monospaced font 
(Monaco or Courier on a Macintosh) to have the graphs and 
tables appear in their proper format.]
Continuation of previous file:

It is time to update our records.
------------------------ Cone 10 Glaze --------------------------
                                                                 
   RO, R2O                 R2O3                   RO2            
(Bases or fluxes)     (Alumina-Neutral)   (Silica - Glass-former)
Mol. Eq. for Fluxes   Mol. Eq. for Al2O3     Mol. Eq. for SiO2   
                                                                 
Max. Lithium   .2  \           .4                        4.5     
Max. Calcium   .65  \                                            
Max. Zinc      .25  / Total                                      
Max. Magnesium .3  / (1.40)                                      
___________                                                      
    1.00    ( <----Remember the fluxes should add up to 1.00)    
-----------------------------------------------------------------

We must now cut our fluxing oxides down to 1.00. The calcium
content is very high, so we will drop .05 off of its molecular
equivalents.  Intuition suggests that zinc and magnesium can cause
the glaze to melt late, muddy the colors, dry out the surface etc,
so we can cut them down to produce the following unity formula of
molecular equivalents:
------------------------ Cone 10 Glaze -------------------------
                                                                
   RO, R2O                 R2O3                   RO2           
(Bases or fluxes)     (Alumina-Neutral)   (Silica - Glass-former)
Mol. Eq. for Fluxes   Mol. Eq. for Al2O3     Mol. Eq. for SiO2  
                                                                
Max. Lithium   .2              .4                        4.5    
Max. Calcium   .6                                               
Max. Zinc      .1                                               
Max. Magnesium .1                                               
__________________                                              
              1.00  Total                                       
----------------------------------------------------------------

If we could fire our test glaze and then reduce a chip from its
surface down to the smallest molecular size which would still
include the correct relationship of fluxes, alumina and silica,
that little atomic or molecular mixture would have the relationship
which we have represented in our last set of glaze notes (above). 

Think of it as if you could focus in on a minute bit of the tiny
molecular trace with an electron microscope and you might be able
to make out some very faint parts in a particular relationship
which would match those we have listed.
_____________   ________________________________________________
|     |/////|   |     |     |     |     |     |     |     |     |
| Li2O|/////|   |_   _ _   _|_   _ _   _|_   _ _   _|_   _ _   _|
| .2  |/////|   |     |     |     |     |     |     |     |     |
|_____|/////|   |_   _ _   _|_                     _|_   _ _   _|
| ZnO |/////|   |     |     |                       |     |     |
|_.1__|/////|   |_   _ _   ___       SiO2 4.5      ___   _ _   _|
| MgO |/////|   |     |     |                       |     |     |
|_.1__|/////|   |_   _ _   ___   _ _   ___   _ _   ___   _ _   _|
|// CaO .6 /|   |     |     |     |     |     |     |     |     |
|///////////|___|__________________    ___   ___   ___   ___   _|
~~~~~~~~~~~~|#####|#####|####|####|     |     |     |     |     |
            |#####|#####|####|####|_____________________________|
                    Al2O3 .4                                     
-----------------------------------------------------------------
A Graphic Image of the Parts (Molecular Equivalents) in our Glaze.

(Please Note: This has nothing to do with real sizes or weights. In
reality, the materials, when melted, would be mixed, helter-skelter
in a glassy, amorphous, liquid-like mix.)
------------------------------------------------------------------

(Step 6.)       Making a Chart Showing the Chemical Molecular
                      Equivalents and the Raw Materials.
                                   or
                     "Getting All of Our Ducks in a Row"
                                                                  
The time has come for us to make the transition from the world of
theory and chemistry to the real world of raw materials which can
be found in nature.  In order to this, we can line our molecular
equivalents up across the top of our page and place corresponding
raw materials down the side. Again, you will need the raw material
information from the Ceramics Gopher at SDSU or from any of the
ceramics texts.

This works out best if you place the fluxes first then alumina and
silica. You may find an easy order by keeping the low-melting
fluxes to the left and working up through the middle and higher
fluxing oxides.
                       / Fluxes or RO,R2O Oxides\/ R2O3 \/  RO2 \
-----------------------------------------------------------------
           Equivalent  |  Li2O | CaO | ZnO | MgO | Al2O3 | SiO2 |
Material     Weight    |   .2  |  .6 |  .1 |  .1 |  .4   |  4.5 |
-----------------------------------------------------------------
Lithium carbonate      |       |     |     |     |       |      |
(slightly water sol.)  |       |     |     |     |       |      |
  Li2CO3       74      |   .2  |     |     |     |       |      |
-----------------------------------------------------------------
Notice that Lithium carbonate is a simple, single fluxing oxide,
material (i.e. It is not combined with other fluxing oxides).
We can use it to supply all of the Li2O in the fired glaze. Note
also that the Carbon (CO3) in the raw material will fire out and
the final glaze will reflect only the oxide relationship of the
lithium.

        Li2CO3 --> Heat --> Li2O
                    ||
                    \/
                  Carbon

Notice we have listed its Equivalent Weight and we will need to
know that in one of the final stages of the process.

Let's continue:

                       / Fluxes or RO,R2O Oxides\/ R2O3 \/  RO2 \
-----------------------------------------------------------------
           Equivalent  |  Li2O | CaO | ZnO | MgO | Al2O3 | SiO2 |
Material     Weight    |   .2  |  .6 |  .1 |  .1 |  .4   |  4.5 |
-----------------------------------------------------------------
Lithium carbonate      |       |     |     |     |       |      |
(slightly water sol.)  |       |     |     |     |       |      |
  Li2CO3       74      |   .2  |     |     |     |       |      |
------------------------- 100% ----------------------------------
Whiting                |       |     |     |     |       |      |
(also called           |       |     |     |     |       |      |
Calcium Carbonate)     |       |     |     |     |       |      |
CaCO3         100      |       |  .6 |     |     |       |      |
---------------------------------100%----------------------------
Zinc Oxide             |       |     |     |     |       |      |
ZnO            81      |       |     | .1  |     |       |      |
------------------------------------- 100% ----------------------
Magnesium Carbonate    |       |     |     |     |       |      |
(slightly water sol.)  |       |     |     |     |       |      |
MgCO3          84      |       |     |     |  .1 |       |      |
-------------------------------------------- 100% ---------------
Alumina Hydrate        |       |     |     |     |       |      |
Al2(OH)6      156      |       |     |     |     |  .4   |      |
---------------------------------------------------100%----------
Silica                 |       |     |     |     |       |      |
(also called Flint)    |       |     |     |     |       |      |
SiO2           60      |       |     |     |     |       | 4.5  |
-----------------------------------------------------------100%--
                       |  100% |100% |100% |100% | 100%  | 100% |
-----------------------------------------------------------------

Before we move on, check to make sure you understand that we are
using the fired or convenient formula to match the raw materials
with the chemical molecular equivalents. The equivalent weight
compensates for the altered formula as it is changed by the fire.
Yet, in our simple (all too simple, I fear!) example the only
changes we see are those of carbon as it is fired out of the glaze.

------------------------------------------------------------------
Raw Material   Raw Formula (nature)    Fired or Convenient Formula
------------------------------------------------------------------
Lithium Carbonate    Li2CO3 ------>     heat ------>     Li2O     
Whiting              CaO    ------>     heat ------>     CaO      
Zinc Oxide           ZnO    ------>     heat ------>     ZnO      
Magnesium Carbonate  MgCO3  ------>     heat ------>     MgO      
Alumina hydrate      Al2(OH)6 ---->     heat ------>     Al2O3    
Flint                SiO2   ------>     heat ------>     SiO2     
                                         ||                       
                                         ||                       
                                         \/                       
                                       Carbon                     
------------------------------------------------------------------

We are almost finished!

(Step 7.)

 Molecular Equivalents X Equivalent Weight = Glaze Parts by Weight
                              or
   (Now That We Have All Our Ducks In A Row, Let Them Multiply.)

While we set our information in order in the form of our molecular
equivalent to raw material chart we also recorded the equivalent
weight for each raw material.  It is time to use all of our
information to move out of chemistry and into the real world where
we can weight and mix the ingredients to make tests of our
empirical work.  Please move to the bottom of this copy of our last
chart .
-----------------------------------------------------------------
                       / Fluxes or RO,R2O Oxides\/ R2O3 \/  RO2 \
-----------------------------------------------------------------
           Equivalent  |  Li2O | CaO | ZnO | MgO | Al2O3 | SiO2 |
Material     Weight    |   .2  |  .6 |  .1 |  .1 |  .4   |  4.5 |
-----------------------------------------------------------------
Lithium carbonate      |       |     |     |     |       |      |
(slightly water sol.)  |       |     |     |     |       |      |
  Li2CO3       74      |   .2  |     |     |     |       |      |
------------------------- 100% ----------------------------------
Whiting                |       |     |     |     |       |      |
(also called           |       |     |     |     |       |      |
Calcium Carbonate)     |       |     |     |     |       |      |
CaCO3         100      |       |  .6 |     |     |       |      |
---------------------------------100%----------------------------
Zinc Oxide             |       |     |     |     |       |      |
ZnO            81      |       |     | .1  |     |       |      |
------------------------------------- 100% ----------------------
Magnesium Carbonate    |       |     |     |     |       |      |
(slightly water sol.)  |       |     |     |     |       |      |
MgCO3          84      |       |     |     |  .1 |       |      |
-------------------------------------------- 100% ---------------
Alumina Hydrate        |       |     |     |     |       |      |
Al2(OH)6      156      |       |     |     |     |  .4   |      |
---------------------------------------------------100%----------
Silica                 |       |     |     |     |       |      |
(also called Flint)    |       |     |     |     |       |      |
SiO2           60      |       |     |     |     |       | 4.5  |
-----------------------------------------------------------100%--
                       |  100% |100% |100% |100% | 100%  | 100% |
-----------------------------------------------------------------
-----------------------------------------------------------------
  Materials            | Molecular  |  Equivalent | Portions by |
                       | Equivalent |    Weight   |    Weight   |
-----------------------------------------------------------------
Lithium carbonate      |     .2   | x |    74     |    14.8     |
Whiting                |     .6   | x |   100     |    60.00    |
Zinc Oxide             |     .1   | x |    81     |     8.10    |
Magnesium Carbonate    |     .1   | x |    84     |     8.40    |
Alumina Hydrate        |     .4   | x |   156     |    62.40    |
Silica                 |    4.5   | x |    60     |   270.00    |
-----------------------------------------------------------------
-----------------------------------------------------------------
Note: Take the Molecular Equivalent times the Equivalent Weight
to get the Parts by Weight.

(Step 8.)  Total the Parts by Weight and Take that Total Into
           Each of the Parts to get a Unity Formula.

With the 'Portions by Weight', you could weigh the amounts and
mix up a glaze test, however, one more simple trick of math will
make you start looking like a professional and give you a unity
glaze recipe (One that adds up to 100) which will make later
testing for colors or correcting flaws like crazing very easy.

All we need to do is add up the 'Portions by Weight' and take the
sum into each of the parts.  It will look like this:
----------------------------------------------------------------- 
Lithium carbonate      |     .2   | x |    74     |    14.8     | 
Whiting                |     .6   | x |   100     |    60.0     | 
Zinc Oxide             |     .1   | x |    81     |     8.1     | 
Magnesium Carbonate    |     .1   | x |    84     |     8.4     | 
Alumina Hydrate        |     .4   | x |   156     |    62.4     | 
Silica                 |    4.5   | x |    60     |   270.0     | 
----------------------------------------------------------------- 
                                        Sum ------>   423.7       
----------------------------------------------------------------- 
          (Round off the figures and move the decimal two places) 
                                                                  
 14.8 divided by 423.70 = .034930375     3.49 Lithium Carbonate   
 60.0 divided by 423.70 = .141609629    14.16 Whiting             
  8.1 divided by 423.70 = .019117299     1.91 Zinc Oxide          
  8.4 divided by 423.70 = .019825348     1.98 Magnesium Carbonate 
 62.4 divided by 423.70 = .147274014    14.73 Alumina Hydrate     
270.0 divided by 423.70 = .637243332    63.72 Flint (Silica)      
------------------------------------------------------------------
                               Unity -> 99.99 (or 100%)           
------------------------------------------------------------------
(Step 9.)  Test it in a Firing if you choose.

Well, there you have it.  A very simple example of the empirical
formula at work to create a glaze.  There are a number of major
problems with our glaze, as you would discover if you chose to
weigh out the chemicals and run a test through a cone 10 firing.
(Remember, we placed some limits on ourselves to keep it as simple
as possible in order to learn about the foundation for the basic
process.

You are probably asking yourself, "What is wrong with the glaze,
it looks like most recipes". You are right, it does have the raw
materials and the weights listed.  It even looks more professional
than many, because we took the time to work it around to equal 100
(Unity). Yet, it can be improved.  Here are some suggestions:

(a) If we could learn how to do the math which will be involved
when we have two or more ingredients coming from the same raw
material, we might be able to cut the number of ingredients down,
or at least, introduce the chemicals into the melt using cheaper
sources from nature.  Raw material sources which contain more then
one material usually enter the melting process earlier and more
evenly.

(b) The alumina, in part or in total, could be introduced in the
form of clay. The clay would keep the glaze from settling out so
quickly in the glaze bucket.  The clay would also provide some
additional dry coat strength, making the freshly glazed surface
less dusty or chalky as it sits on the shelf waiting for the next
firing. Of course clay would also help provide some of the silica
which will be needed in the mixture.

You may run a test of the glaze, just the way it appears here,
however, in a later lesson, we will learn to use more complicated
raw materials which will help us overcome some of the problems
which resulted from choosing the simple, single material, oxides.

As we end this lesson, some brief remarks concerning the process
of testing a base glaze for color response.  We did the work and
have our glaze adding up to 99.99 (100.)   In a situation like
this, where they are one or two tenths lower or higher then 100,
most of us just add or subtract a tenth or two for one of the
ingredients. (Here, silica is in the largest quantity, so by
adding one tenth to its total, we have no effect on the finished
melt.   The alternative is to round the numbers until the total
comes to 100.

 3.49 Lithium Carbonate   ------->  3.5       3.49            
14.16 Whiting             -------> 14.2      14.16            
 1.91 Zinc Oxide          ------->  1.9  or   1.91            
 1.98 Magnesium Carbonate ------->  2.0       1.98            
14.73 Alumina Hydrate     -------> 14.7      14.73      from  
63.72 Flint (Silica)      -------> 63.7      63.73 <-- (63.72)
--------------------              ------     ------           
99.99 (or 100%)                -->100.0  -->100.00            
--------------------------------------------------------------
(Step 10.)  Run Line Blends to Find its Color Response, Correct
            Flaws or Change the Surface.

The advantage of working the formula around to equal 100 makes it
very easy to run line blends in the next phase of testing. After
the base glaze is tested and has proven to merit additional work,
you will want to see what kind of color response it will yield.
Each test can be thought of as a percentage relationship to 100
parts (Unity) in the base glaze. For example: A typical line
blend for a base glaze test for color response to cobalt would
look like this:

Test #          1     2     3      4     5      6     7      8   
Base Glaze    100.   100.  100.   100.  100.   100.  100.   100. 
Cobalt Carbonate .25    .50   .75   1.    1.25   1.50  1.75   2. 

Most of us would speed the line blend up a bit by making four
simple tests of .25, .50, 1.,and 2. grams for each 100 gram lots.
(You can always go back and test between the weights if you need a
specific adjustment to the color between two tests.) We should note
that it is very hard to get an accurate test of .25, or .50 grams.
The logical way to test for very tinny amounts is to double both
the base amount and the metal color oxide. So a test of 200 grams
of base with one gram of cobalt would be the same as a test of 100
grams of base and 1/2 (.50) gram of the metal but the result of the
larger quantities would be much more accurate if you are using a
gram scale.  Many of the standard texts for ceramics include
varying suggested limits for metal oxides used to produce color in
the melt.  A quick glance at any of those charts will help you get
started with the planning stage for color line blend tests.

I have found the most productive limits for metal oxides for glaze
color are as follows:

Cobalt Oxide and Cobalt Carbonate   00.25%   -------->  2%       
Red, Black, and Yellow Iron Oxide    1.00%   --------> 11%       
Iron Chromate                        1.00%   -------->  5%       
Copper Carbonate and Copper oxide    1.50%   -------->  6%       
Chrome Oxide                         1.50%   -------->  5%       
Manganese Dioxide                    1.00%   -------->  5.75%    
Nickel Oxide                          .50%   -------->  3.50%    
Ilmenite                             1.00%   -------->  4.50%    
Rutile                               1.00%   --------> 10.00%    
Vanadium Pentoxide                   4.00%   -------->  9.50%    

Your best bet is to run two or three sample percentages distributed
throughout the total range for each metal oxide, then after those
tests come from the kiln, you can decide on the best use of your
time in the next round of tests.

Blacks result from the saturation of the glaze with metal, so
try using two or three metals in quantities from 1% to 5%. Saturate
Iron glazes usually have 8% to 10% added to the base. Iron becomes
a more active flux in reduction and Manganese fluxes more in an
oxidation firing. Try to avoid large quantities of cobalt.  This
will cause the glaze to become very fluid. Chrome and Nickel will
dry and matt the glaze surface.

Some of your bases will come from the first test firing with an
acceptable matt, opaque white.  Other glazes can be made white
with tin, titanium or zirconium silicates.  Tin is one of the
most expensive choices for white, although it has a variety of
soft and unique effects on other coloring oxides.  The Zirconium
silicates will usually produce a strong or harsh, "Bathroom Bowl"
quality of white which works well as a uniform support for strong
brush work contrast. The limits for most of the opacifiers are in
the range of 5% to 11%.

-----------------------------------------------------------------

Lets review the steps we used in this lesson:

(Step 1.)  Choosing a Maturation Temperature


(Step 2.)  Finding the Average Molecular Equivalents For Silica
           at Cone 10

(Step 3.)  Finding the Average Molecular Equivalents For Alumina
           at Cone 10

(Step 4.)  Choosing the Fluxing Oxides

(Step 5.)  Finding the Molecular Limits for the Fluxes

(Step 6.)  Making a Chart Showing the Molecular Equivalents
           and the Raw Materials.

(Step 7.)  Take Molecular Equivalents Times the Equivalent Weights
           in order to get the Glaze Parts by Weight

(Step 8.)  Total the Parts by Weight and Take that Total Into
           Each of the Parts to get a Unity Formula.

(Step 9.)  Test it in a Firing if you choose.

(Step 10.) Run Line Blends to Find its Color Response, Correct
           Flaws or Change the Surface.
-----------------------------------------------------------------
(c) 1994 Robert Fromme           For educational use, only.
-----------------------------------------------------------------



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