A little update, work continues

Work continues on silver stain. It's been my primary focus for the past few weeks. Tonight, after my birthday dinner, I started grinding some brick dust to try as a binder:

A little research suggests that before the 14th century almost all brick was what we'd call terracotta. I bought a small terracotta pot, set it on a ledge, and aimed a laser pointer at it. Gravity and a cat with a hair trigger gave me shards to grind into my dust. For testing my various binders (What was mostly planned to be "part 1"), I've been using silver nitrate and each binder (1:6). For what I meant to be my compound tests ("part 2") I've been using gum arabic. I've found no indication that it is a period binder for this purpose, but I trust it not to fire onto the surface of the glass.

Copper Sulfate is supposed to give an amber color to the glass. It's proving difficult and I think I will have to try it at a higher temperature. Silver sulfate and silver nitrate are both working as expected. I've purchased some "name brand" red ochre to try again; the 'generic' stuff I used before appears to be way off and now the line between phases of my project is quite blurred.

I'm presently up to four binders, three of which are mentioned in the period formula, and four compounds, one of which is mentioned in the period formula. Once I have some confidence in the binders I will smash up the materials needed to actually try the period recipe.

Silver Stain Experiments pt 1

I've become fixated with the idea of making and controlling my own silver stain. I particularly want to do it following a period recipe to enter into A&S.

[Edit 9/6/13: I'd like to clarify that this "Phase 1" is about finding the right binder. Phase 2, detailed at the end but not well explained, is about finding the right silver and copper compounds to create various colors. Phase 3 is actually using the period recipe.]

After a considerable bit of research I've only been able to track down one recipe, which calls for antimony sulfide and silver in a liquid suspension, diluted 1 part to 6-10 parts by some form of clay (brick dust, ochres, etc). [This book, p. 11]. Antimony sulfide, also called stibnite, is not especially safe since it's an antimony compound. The recipe from that book, incidentally, supposedly comes from one (of many) versions of the Lapidario of Alphonso X (Alphonso the Wise). I've gotten a copy of that specific version, but no English translation is available and automated translations were insufficient for me to pick out the recipe. Fortunately somewhere in my skull is 4 years of Spanish. I am working on translating the document and finding the recipe from this primary source.

A brief aside, I was pointed at the Mappae Clavicula by Master Ali. A latin copy was available and, working with a dictionary, I thought I found another recipe. After I ordered an English translation I discovered a slight error with a big impact. It is still an awesome text with amazing recipes, including many glass-related ones!

Modern silver stain is made using silver nitrate, silver sulfate or (for dark stains) copper sulfate [This book by J. Kenneth Leap] in a binder (various clays or gums will work). For the first round of experimentation I decided to try and make a half-way modern stain to start with, eliminating the least safe part until a later time when I can use a fume hood and better safety equipment.

My "round one" experiment was to use purchased silver nitrate (AgNO3), combined with the binder in the period formula at a ratio from the period formula. I bought two grams of reagent grade silver nitrate online for $10 including shipping [Here]. I ordered yellow and red ochre pigments online as well [Yellow: $6 inc. shipping for 30 grams by Vallejo Pigments; Red: $15 inc shipping for one half-pound of unspecified provenance].

The first step was grinding the silver nitrate. It comes in small crystals in a small amber vial (it's a photosensitive compound, I understand). I used a mortar and pestle, as well as a small disposable brush:

Crushcrushcrush isn't just a song by Paramore...

2 grams yielded considerably more powder than I expected. I used a small-unit digital scale to measure out 2 1-gram portions of the silver. Unfortunately it didn't go further, so I divided each portion into quarters as best I could visually. My primary goal with this was to see if it would even work or if I were missing some other "secret sauce". I then used the scale to measure out grams of ochre to reach the desired strengths. In the spirit of what I'm doing, I mixed the ochre and silver nitrate in a handmade bowl Master Ali ("Arab boy") generously gave me at Pennsic when I went to pick his brain about alchemical implements:

An academic article I found indicated that red and yellow ochres should inhibit the silver ion exchange (for more info, see the Leap book referenced above) that makes silver stain work. The reason is that the iron content in red ochre affects the transfer [Academic article can be found here. For details from it, email me at Brynn dot Herleifsson at gmail dot com]. The article, and several others, was kindly provided by a friend with access to those digital libraries, saving me the considerable expense.

I mixed three batches. The first was mistakenly made weak, 1 part AgNO3 to 16 parts yellow ochre. I decided to keep it and do a 1:16 batch using red ochre. I then made a 1:10 batch using red:

It was a little uncomfortable making lines of various white and colored powders on a digital scale. Just sayin'....

I made small batches of each mix in my usual method (with oil, as I learned from these gentlemen). For a "proper" batch I'd mix it with sandalwood amyris oil, and dilute it for use with lavender. Lavender is lighter, and I wanted the chips to dry faster, so I only used that.

The 1/16 yellow ochre blend, mixed with lavender oil 

The 1/16 red ochre blend, with lavender oil. The 1/10 mix is identical, no photo taken

I put some stain on three test chips and blended them as I normally would. The 1/10 red mix was difficult to blend, but I attribute that to being slightly too dry. My purpose was to see if it would even work, so I moved ahead rather than keep blending (Preparing the chips, the mixing, staining, and starting the kiln were done in the span of my lunch break from work). I used a glass that I've stained before, so I knew it would take without difficulty unless the batch were bad.

The three test chips on whitening, before firing

I fired them at my usual silver stain schedule (also one provided by Williams and Byrne, available here but to summarize.... 212°/hour to 212°, 570°/hour to 1000).

Hours later, I was rewarded:

I've color-corrected this picture to the best of my abilities. The top and right chips are a little too muddy yet, in reality they are just a bit more darker/amber than the other. They also have some residue, detailed below

[Edit 8/28 Afternoon: I have a stronger test chip in the kiln right now, but while walking past my lightbox I realized that a picture taken from an angle shows the color differences between the red and yellow mixes a little better. It's still not perfect, my eyes pick up more differences than my camera:

]

The un-stained portions are from imprecise handling during blending. The bottom two are the 1/16 mixes, the top the 1/10. Right and top are red ochre, left is yellow ochre.

[Edit 8/29] I decided I needed to try a stronger mix right away, my excitement was distracting. I mixed a 1:6 strength batch with red ochre and fired it today. Unfortunately the results were very disappointing. The chip appears to have even more nasty residue than the others. I'm not sure if red ochre itself makes for a poor binder, or if my particular supplier is unsuitable. I wish I had powder left so that I could try a stronger batch with the yellow ochre, which is the only test chip with no residue. The new one is bottom-right in this picture:

The stain is not brown or amber, there is a hazy shmutz all over the glass, and very little yellow tone. This is the same glass as the other three pieces.]

Lessons Learned and Observations

• I have one glass palette I use for small batches, tests, etc. I opted for it because I never bothered to sand it. This makes for easier ("more scientific") clean-up and, I hoped, less contamination between mixes. Unfortunately it also made it very difficult to get a good mix!
  
• I find alchemy texts and experiments FREAKING COOL. That counts as a lesson learned.
• I do notice a difference between the red and yellow ochre mixes, however I'm not convinced it isn't due to handling issues. It looks like I got more of the red mixes onto their test pieces, they were quite thick compared to the yellow after I blended them. I will need to try and find a very controlled way to compare them to see if the journal article pans out in practice. This is especially visible in the graininess of the yellow sample above (bottom/left).
• Red ochre powder is a beautiful substance and a wonderful pigment. It's also a beast to clean up. The chips have what I'd almost swear is fired-in ochre on their surfaces, making them look less clean when viewed close up. I'm not sure what the source is. The palette I used last had "red for flesh" mixed on it, and I had just cleaned it off before mixing the silver stain. The residue looks convincingly like RfF:

A shot of the 1/10 red ochre test chip using reflected light to show the residue on the "inside" (unstained) surface

Next steps

Phase 2 (Sept/Oct) -

• Try a 1:6 ratio mixture with yellow and red ochres, the strong end of the range given above.
• Try to keep it very clean and even to compare the effects of the binders
• Try mixtures with silver sulfate, copper sulfate, and mixes of the three compounds.
• Try mixtures including brick dust, gamboge gum, and other substances as the binder.

Phase 3 (Nov/Dec) -

• Try the actual period recipe, involving stibnite (already acquired) and silver
• Try a syncretic recipe involving a period recipe for nitric acid (aqua fortis) and silver, resulting in a modern formulation made using entirely period techniques (Assuming that they didn't use that same formula, but there doesn't appear to be any existing document indicating as such. The (al)chemical knowledge was completely in place to do so, however). Maybe Roana can use some of the acid for her book binding as well?

A&S50 #6: Device of Alexander Adelbrecht von Markelingen [In Progress]

I received a lot of great feedback from Moll at Pennsic after she looked over a few of my pieces. One was that I need to use matting more and rely less on my tracing paint. I wanted to practice more, so I referred to a file I keep with close friends' devices and badges. My SCA-nephew Alexander's device was perfectly suited for this:

I laid down some matting paint in the chief and in the center, and cut down a cheap brush to use as a scrub. I scrubbed the antler out of the chief and fixed the shape of the heart, then took this photo.

Before firing it, I continued to clean up the shape of the heart, the erminois spots, and the final point of the antler. I fired it and was going to let that be the end of this one, until a few days later. I am working on learning and designing decorative techniques to go around glass heraldry. The idea occurred to me to surround it with glass, give those pieces a brown matt, and scrub out ermine spots as diapering. I think this one will develop further into a more complete panel.

This also came from the thickest batch of paint I've mixed yet. I think I added too much gum arabic, as this clings powerfully. I remember a twitch in my wrist while sprinkling on the gum, and thought I'd let it go and see how it ended up. It's functional, but a little difficult. The "freshly fallen snow" amount was more like "freak snow storm" in this case.

Another thing I noticed is that the scrubs I use, hog bristle, tend to leave thin lines behind in the removed area. A second pass easily removes them, but I find the look very appealing. It reminds me of woodcarvings and prints made by hand. It's a rare example of a time when I prefer an imperfection. I don't know how much of that I can get away for A&S or commercial standards, but I like it. I decided to leave some of the marks visible in the antler on this piece as a result.

#4: The Arms of the Barony of White Waters

So, since I've decided to combine my long-term goal of doing the Baronial arms of all 19 Midrealm baronies, and competing in A&S 50, I need to get a move on. This weekend is Swine and Roses, hosted by the Barony of the White Waters. Rather than do the devices in order of precedence, I've always planned on doing them in order of proximity to me. Having the closest ties to White Waters, and the first "deadline", they are first up.

Azure, a mullet of four points within a laurel wreath Or, a chief wavy argent.
 
Cutting the mask was a major pain in the fingers. I cut the escutcheon from blue-flashed-on-clear, and applied three stripes of Gorilla duct tape. A very thin coating of wood glue, and then my paper copy of the baronial arms. After it dried, I attacked it with an X-acto knife. Peeling the pieces out was a challenge, and today I ordered a set of steel dental picks.

Four pictures taken while removing the mask:

The acid etching began last night [8/13/13]. The panel needs to be completed for submission at S&R on the 17th.

[Edit 8/19/13]

The acid etching wasn't going quite fast enough. I realized the panel would probably be done Sunday, but I needed it Friday evening to stain. Mistress Kirsten shared with me a copy of her documentation a few years ago, and while I don't have her sources, yet, I know from her that abrasion is a period way to remove flashed glass. I've manually removed flashed glass with an "engraving point" for my dremel, and it's a very slow process. It's not well-suited for the space I needed to clear and the time I had. I did this with my dremel on a low speed:

It's very pretty, and the glass was left with a nice texture. I started to silver stain it, and had a problem. Due to the detail level it became very hard to remove excess stain after I blended it. It would probably have been much easier if I had waited until the stain dried and could have scratched it out. I was working with Q-tips, paper tower etc. and found it almost impossible. I removed too much frequently, trying to clean up the stem:

It was 3 AM and I needed sleep, so I gave up on the idea of entering it at Swine and Roses. On my drive there the idea occurred to me to fire it in three stages. Once for the mullet (4-pointed star) and the stem of the laurel wreath, once for half of the leaves, and once for the other half of the leaves. This would let me have plenty of wiggle room to clean up and detail the stain after blending. I'm not sure whether the results would be better when compared to waiting for it to dry and scraping it with a stick. That may require some experimentation.

[Edit 6/12/14]
Yow! I never updated this post. Here is the roundel >.<

Midrealm Populace Badge

Post-in-progress! Come back for more.

The "Midrealm takes care of its own" mini-event at Crown is in full-swing. I pledged two pieces of glass work, but wanted to goad my household into contributing as well. I told them if five of them contributed an item to the silent auction, donated to the cause, or gave an item for the bake sale, that I would also give a celtic knotwork piece I found. If 10... I would do the Midrealm Populace Badge.



I found a beautiful Welsh Dragon pattern at this website and realized it could be easily modified for Midrealm usage. It's a straightforward modern work, about 24x18. I hope to put it in an oak frame as well.

 At this point I realized three of the pieces were darker than the others in this photo, while discussing it on Facebook. I came to find out that I had grabbed a nearby sheet of red that was different, and recut them in the right glass.

The following pictures were taken as I fit the pieces into my soldering jig. The green appears almost black, the photos losing some of their beauty.

Finished pictures and silent auction results to be announced after this weekend!

[Edit 5/30/13: I ran out of solder! Ye GADS! I used the picture below to enter the panel into the auction, where it brought in a respectable sum for the cause.]

Next update will be final, with a shot of it cleaned up, patina'd, and framed.

[Edit 7/8/13] Below is a shot of the final panel, just before delivery. Not 100% happy with it, but it needed to get delivered.

Paint chips

Paint chip samples, to go into the binder. Before firing they always look lifeless and like drawing pastels, in reflected light:

Pre-firing, in transmitted light. I sketched little phrases on them for contrast. The samples are intentionally not blended even:

This was a very beneficial test, in the end, because the transparent green enamel I thought I bought was opaque. That project got sidelined for a bit as I try to decide whether to try it with enamels, or flashed glass. I don't want a leadline where... ah, but that's another post for another day. Three new colors coming this week to test as well.

Pennsic Lantern

I want a nice-looking light source for Pennsic, although I'm going to keep it modern and electric. I have a thing for lanterns, but the two hanging for decoration around the house (with LED candles) aren't suitable for.... <evil Russian accent> Enhancement....</accent>. This made for a nice, and quick project.

I was passing through Menards and found these decorative lamps on sale, with a hinged door, for $10. I opened it up and immediately saw the four glass panes are held in by bendable metal tabs.

 

I took it home and bent out the tabs to discover that the pieces are also held in place by a strip of foam adhesive, kind of like what you'd mount a poster with (if you had no regard for the quality of the posters). My plan was to replace the two side panes with Midrealm Pales and the door (back) with mirror, to channel the light out the front. So, with that in mind, I took my glass cutter, scored horizontal lines across them, and smashed out the glass.

I used pliers to remove the shards and the foam adhesive strips. Then I cut strips of glue chip glass. I don't want lead lines impeding the light coming out of the lanterns, so I laid them on my lightbox and used a clear silicon adhesive/sealant to glue them together.

I cut a piece of mirror for the door and glued it into place, along with squares for the inside ceiling and floor, again to channel the light.

Once the silicone sealant was solid enough, I popped the panes into the sides and closed up all the tabs. Lantern done! I intend to take a bright flashlight and put it in the lantern, possibly rigging a switch near the handle on top.

Test Binder

A helpful idea to share quickly. I've begun accumulating test pieces and samples to the point where I can't keep them straight anymore. Enter my test binder:

I took an old binder, and filled it with baseball card sleeves you can get at your local hobby shop or Wal-Mart (try the hobby shop first). Each glass chip goes into a sleeve, with the back of a piece of 3x5 notecard. This gives an even white surface for viewing the samples, and the lined side of the cards has notes on what the sample is. Right now I have a description and, when relevant, firing schedule for each piece recorded.

Memorial Disks

After several weeks of not being able to stand at my work benches (sprained ankle followed by gout attack), and with very few weeks until my last option to enter MK A&S for the year, it's time to put the hammer down and get serious, or I won't be entering this year at all.

It took a dozen tests to get everything settled, to get a method to create two armorial disks. The disks are bearing the arms of a departed friend, blazoned "Azure, a chevron argent, overall a Latin cross Or." One will go into a panel for A&S. One will be attached to the lid of the handmade box containing his ashes.

I ordered two square feet of flashed glass, blue-on-clear. I also had a small (7x7") scrap of blue I found on a fluke at a local shop that doesn't normally carry flashed. I placed that into my Morton circle cutter and popped out a perfect disk. For the second disk, I cut one of the new sheets up. Popped it into my circle cutter, and met with heartbreaking (and expensive) disaster as the disk mis-cut. A second square became two more half-circles. Then a third. I blew through $75 worth of glass in an hour. I decided to forgo the fancy circle cutter and do it slowly, by hand and grinder.

Not too bad. Then, on to the acid etching. Resists/masks have been a problem for me, after several tests. Duct tape (fuzzy edge), contact paper (very fuzzy edge), and a resist gel were tried and found problematic. Most of the "tape" solutions I was trying are actually suggested for sandblasting flashed glass, not acid-etching it. I tried them anyway, because I had no better ideas and I'm not yet equipped for sandblasting. The gel was especially tricky because after I smeared a coat on the glass, I needed a "resist resist" to keep clear my target pattern. I laid down duct tape first, and lifted it to try and leave behind what I needed, but the lines weren't clear enough for my taste.

I ended up going back to duct tape, figuring I'd rather have a roundel with slightly fuzzy edges than none at all. I wanted a wider roll, however, to avoid issues where two pieces of tape match. A trip to the hardware store turned up a 4" wide roll of Gorilla-brand tape... and this stuff is mighty. I put a strip of Gorilla tape mostly across where the design will be, and two extra strips above and beneath. I then covered the gaps with two more thin strips, trying to get as much coverage as possible. I put a copy of the roundel on top with white glue, attacked it with an X-Acto knife, and got something workable.

Then, began the cycles of acid etching cream. Five of them, I do believe, in all. Sitting on scrap mirror for protective purposes:

After two coats, I believe:

Three coats:

 

After four:

 

I was shocked but pleased with the result. I gave it a fifth coat to clear up the edges. The glass is a lot clearer than I expected, more so than with sandblasting. While washing it in the end the water filled in the pits and made it completely clear.

The Gorilla tape worked far, far better than I had hoped. It stood up to wirebrushing to remove dried coats of acid etch, and kept the fine points intact. Here is a shot on top of my ancient crown template, for visibility.

Now knowing how to get the silver stain to work, I applied my stain and fired it.

I am exceedingly pleased with the result!!! Now, to get it into a panel....

Painting Practice Pieces

I made a quick practice piece to check my firing schedules and the paints:

For some reason (other than being an SCA herald?) I like to use an Ancient Crown for my practice pieces. I mixed a small batch of Reusche 1059 tracing black, and a matting color of about 50/50 Reusche 1220 A gray green and 1110 bistre brown #7. I did the matte, waited, very roughly traced the ancient crown, waited. I removed the matte from about 2/3 of the crown and did a thin highlight around the entire border. Fired it, applied the silver stain, tried a new blender, and fired. This shot shows some of the matting coming off:

 I'm using Reusche 1384 silver stain, Yellow #3. I had a previously mixed batch. I took a small bit, diluted with lavendar oil, and diluted it too much. Then I kept putzing about with it, and it was too dry when I went to hit it with the blender. Eh, I thought, it's a test piece. Fired it again:

 I am not unhappy with it. The matting is too light, the lines irregular and poorly traced (but it was a test piece), and the silver stain uneven. The only actual problem I've noticed is metalling where my silver stain is thicker. It happened once before, as well:

 

I checked my firing schedule (I'm using schedules from Williams & Byrne), and I noticed that my current schedule only goes to 1040°. Metallizing, as I understand it, normally happens when you fire too hot. RP 1384/Silver Stain, Yellow #3 has a listed firing range of 1050-1080. I'm going to do two more tests this week, firing to 1020° (20° below my current schedule) and 1060° (20° above) to see what the effects are. Viewed directly on the stain is pretty, this may be something I end up having to live with, because I can't image 30 degrees below the listed range is going to make it better, and going higher should make it worse if this is actually metallizing.

(Update, 4/17/13)

I ended up with interesting results. The test piece fired to 1060°, just inside of the manufacturer's listed range, turned out horrifically bad. I went ahead and fired it on a chip with a blue enamel I have plans for, and this was my result:

Horrible metalizing, "yellow mother-of-pearl" as I expected from Williams & Byrne's books, their description of overfired silver stain. It looks horrible in both reflected and transmitted light.

The chip fired to 1020° was relatively the same as 1040°:

Looking straight through it, its functional, but there are some off spots and in reflected light you can see its still not right. Thirty degrees beneath the listed range, and it's still not right? I started to suspect I was firing for too long, then, because surely it couldn't be too hot...

Checked Elskus, seeing what he had to say on the matter. Silver stain, according to him, has a functional range of 950° to 1050°! I'm still on the high end, according to him. Ok, one more chip, at 1000° then.

This picture doesn't do it justice. Beautiful and quite even. I stared at the chip for several minutes, held it up to various lights, placed it on my lightbox. I put it by my computer and picked it up ever few minutes for an hour, staring. 1000° it is, then, and that temperature has been working great for me. As the masters wrote and write, experiment and experiment some more...