Dear Walter, I am doing similar treatment for silanization but I am using different process for cleaning glass substrates. I have not used piranha solution but hot NaOH and ultrasonication for cleaning. Is that a problem? In addition, after silanization with (3-trimethoxysilyl)propyl methacrylate (TMPMA) do I have to see opaque layer on the surface of the glass or the glass is completely trasparent?
Dear Walter, I am doing similar treatment for silanization but I am using different process for cleaning glass substrates. I have not used piranha solution but hot NaOH and ultrasonication for cleaning. Is that a problem? In addition, after silanization with (3-trimethoxysilyl)propyl methacrylate (TMPMA) do I have to see opaque layer on the surface of the glass or the glass is completely trasparent?
Hello Prof Walter J Dressick and all, I just wanted to know that what happened if the water is 2Mega-ohm deionized and after cleaning the glass with Dressick's protocol , is it right to do silanization with ethanol solution. Can you tell me the further protocol for silanization with ethanol? @Walter J Dressick
Hello Prof Walter J Dressick and all, I just wanted to know that what happened if the water is 2Mega-ohm deionized and after cleaning the glass with Dressick's protocol , is it right to do silanization with ethanol solution. Can you tell me the further protocol for silanization with ethanol? @Walter J Dressick
If this discussion is active still, could someone let me know how we may confirm that the monolayer of APTES on the glass slide is uniform. In the papers below,
(1) Nath, Nidhi, and Ashutosh Chilkoti. "A colorimetric gold nanoparticle sensor to interrogate biomolecular interactions in real time on a surface." Analytical chemistry 74.3 (2002): 504-509.
and
(2) Nath, Nidhi, and Ashutosh Chilkoti. "Label-free biosensing by surface plasmon resonance of nanoparticles on glass: optimization of nanoparticle size." Analytical Chemistry 76.18 (2004): 5370-5378.
it has been mentioned that the glass slides must be sonicated 5 times in ethanol. However, every time, I see a white-colored precipitate on the glass slide after the 3 hr, 120 deg C drying step. While following this step, I see gold nanoparticle aggregates on the surface, even if I sonicate the colloidal sample prior to deposition. It must be noted that I used microscope glass slide instead of cover glass slide. I would like to know why "cover glass slide" is preferred to "microscope glass slide" for chemisorption of gold nanoparticles?
If this discussion is active still, could someone let me know how we may confirm that the monolayer of APTES on the glass slide is uniform. In the papers below, (1) Nath, Nidhi, and Ashutosh Chilkoti. "A colorimetric gold nanoparticle sensor to interrogate biomolecular interactions in real time on a surface." Analytical chemistry 74.3 (2002): 504-509. and (2) Nath, Nidhi, and Ashutosh Chilkoti. "Label-free biosensing by surface plasmon resonance of nanoparticles on glass: optimization of nanoparticle size." Analytical Chemistry 76.18 (2004): 5370-5378. it has been mentioned that the glass slides must be sonicated 5 times in ethanol. However, every time, I see a white-colored precipitate on the glass slide after the 3 hr, 120 deg C drying step. While following this step, I see gold nanoparticle aggregates on the surface, even if I sonicate the colloidal sample prior to deposition. It must be noted that I used microscope glass slide instead of cover glass slide. I would like to know why "cover glass slide" is preferred to "microscope glass slide" for chemisorption of gold nanoparticles?
I have been making self-assembled organosiloxane monolayers for 25 years. The cleaning method I use is: (1) Soak glass slides in a solution comprising one volume of concentrated HCl and one volume of methanol for at least 30 minutes (longer times are OK) to degrease the surface. (2) Rinse the slides THOROUGHLY (at least 4 times) with 18.2 Megaohm-cm deionized water. (3) Soak the slides in concentrated sulfuric acid for at least 30 minutes (longer times are OK). (4) Rinse the slides thoroughly (at least 4 times) in 18.2 Megaohm-cm deionized water. (5) Place the clean slides in gently boiling 18.2 Megaohm-cm deionized water for 30 minutes. (6) Remove the slides from the gently boiling water and dry them thoroughly using filtered nitrogen gas from liquid nitrogen boil-off. (7) Place slides in the organosilane treatment solution. This method has produced reliably clean slides for monolayer deposition for me. It avoids the use of dangerous piranha solutions as cleaning agents. The rinse step in step (2) is very important. If all the HCl-methanol is not removed, the sulfuric acid will react with it to leave a deposit on the glass surface. Do not use compressed nitrogen gas from tanks in step (6) because it may contain trace oil from pumps used to fill the tank that would deposit on the clean glass. The cleaning process described is thought to maximize the surface Si-OH concentration for monolayer deposition.
I have been making self-assembled organosiloxane monolayers for 25 years. The cleaning method I use is: (1) Soak glass slides in a solution comprising one volume of concentrated HCl and one volume of methanol for at least 30 minutes (longer times are OK) to degrease the surface. (2) Rinse the slides THOROUGHLY (at least 4 times) with 18.2 Megaohm-cm deionized water. (3) Soak the slides in concentrated sulfuric acid for at least 30 minutes (longer times are OK). (4) Rinse the slides thoroughly (at least 4 times) in 18.2 Megaohm-cm deionized water. (5) Place the clean slides in gently boiling 18.2 Megaohm-cm deionized water for 30 minutes. (6) Remove the slides from the gently boiling water and dry them thoroughly using filtered nitrogen gas from liquid nitrogen boil-off. (7) Place slides in the organosilane treatment solution. This method has produced reliably clean slides for monolayer deposition for me. It avoids the use of dangerous piranha solutions as cleaning agents. The rinse step in step (2) is very important. If all the HCl-methanol is not removed, the sulfuric acid will react with it to leave a deposit on the glass surface. Do not use compressed nitrogen gas from tanks in step (6) because it may contain trace oil from pumps used to fill the tank that would deposit on the clean glass. The cleaning process described is thought to maximize the surface Si-OH concentration for monolayer deposition.
Does concentrated nitric acid work equally well in place of conc. sulfuric acid here? Also, has anyone tried more dilute (1M) acid at longer intervals for cleaning/activation?
Does concentrated nitric acid work equally well in place of conc. sulfuric acid here? Also, has anyone tried more dilute (1M) acid at longer intervals for cleaning/activation?
Dear Dr. Vu: Mix 1 volume of concentrated (12 M) HCl and one volume of pure methanol- add the HCl carefully with stirring to the methanol. For the sulfuric acid, use concentrated sulfuric acid directly. Rinse substrates well with deionized water after removal from each of these acid solutions.
Dear Dr. Vu: Mix 1 volume of concentrated (12 M) HCl and one volume of pure methanol- add the HCl carefully with stirring to the methanol. For the sulfuric acid, use concentrated sulfuric acid directly. Rinse substrates well with deionized water after removal from each of these acid solutions.
Add the methanol to a beaker and initiate stirring. Slowly pour the HCl down a glass stir rod into the stirring methanol (i.e., add the HCl slowly to the stirred methanol. Do NOT add methanol to a volume of HCl to avoid local superheating and splashing). Work in a well-ventilated fume hood. Wear safety eye goggles, a lab coat, and gloves. Consult the MSDS forms for methanol and HCl for any other hazards and safety information BEFORE beginning.
Add the methanol to a beaker and initiate stirring. Slowly pour the HCl down a glass stir rod into the stirring methanol (i.e., add the HCl slowly to the stirred methanol. Do NOT add methanol to a volume of HCl to avoid local superheating and splashing). Work in a well-ventilated fume hood. Wear safety eye goggles, a lab coat, and gloves. Consult the MSDS forms for methanol and HCl for any other hazards and safety information BEFORE beginning.
It would be nice of you if I can have your opinion regarding my experimental silanization process. I am using the Piranha cleaned glass substrates (contact angle 5°, after Piranha cleaning) for the silanization process. The silane I am using is N-trimethoxysilylpropyl. I add 1 mL of silane into 50 mL of de-ionized water and heat the solution with magnetic stirring at 80°C for 30 mins. After that I rinse it with extensive water for 30 mins and gave supersonic bath treatment for 30 mins. and dried under vacuum for 1 h. But unfortunately, the glass substrates were not rendered hydrophobic. I observed the contact angle of only 30° after silane treatment. Can any body help/suggest me in this regard?
It would be nice of you if I can have your opinion regarding my experimental silanization process. I am using the Piranha cleaned glass substrates (contact angle 5°, after Piranha cleaning) for the silanization process. The silane I am using is N-trimethoxysilylpropyl. I add 1 mL of silane into 50 mL of de-ionized water and heat the solution with magnetic stirring at 80°C for 30 mins. After that I rinse it with extensive water for 30 mins and gave supersonic bath treatment for 30 mins. and dried under vacuum for 1 h. But unfortunately, the glass substrates were not rendered hydrophobic. I observed the contact angle of only 30° after silane treatment. Can any body help/suggest me in this regard?
There are many ways to clean glass for such experiments. People generally saturated KOH, piranna etch or NH4OH, H2O2 and HCL. KOH treatment and plasma cleaning renders glass hydrophilic we compared different chemical treatments on glass at nanometer scale here using Atomic force microscopy ArticleGlass is a Viable Substrate for Precision Force Microscopy o...
There are many ways to clean glass for such experiments. People generally saturated KOH, piranna etch or NH4OH, H2O2 and HCL. KOH treatment and plasma cleaning renders glass hydrophilic we compared different chemical treatments on glass at nanometer scale here using Atomic force microscopy ArticleGlass is a Viable Substrate for Precision Force Microscopy o...
I don't know what "opac" layers are. After the RCA treatment, the glass is clear and completely wetted by water. I have not used an acrylate silane for chemisorption. If you see a film after chemisorption, it probably means you have a multilayer formed by silanol and/or vinyl group polymerization. In that case, you need to experiment and change your chemisorption conditions to get a uniform monolayer film (if that is what you are trying to make).
I don't know what "opac" layers are. After the RCA treatment, the glass is clear and completely wetted by water. I have not used an acrylate silane for chemisorption. If you see a film after chemisorption, it probably means you have a multilayer formed by silanol and/or vinyl group polymerization. In that case, you need to experiment and change your chemisorption conditions to get a uniform monolayer film (if that is what you are trying to make).
I would go for piranha cleaning for 20 mins which should be enough for for silanization
I would go for piranha cleaning for 20 mins which should be enough for for silanization
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Dear Walter, I am doing similar treatment for silanization but I am using different process for cleaning glass substrates. I have not used piranha solution but hot NaOH and ultrasonication for cleaning. Is that a problem? In addition, after silanization with (3-trimethoxysilyl)propyl methacrylate (TMPMA) do I have to see opaque layer on the surface of the glass or the glass is completely trasparent?
Dear Walter, I am doing similar treatment for silanization but I am using different process for cleaning glass substrates. I have not used piranha solution but hot NaOH and ultrasonication for cleaning. Is that a problem? In addition, after silanization with (3-trimethoxysilyl)propyl methacrylate (TMPMA) do I have to see opaque layer on the surface of the glass or the glass is completely trasparent?
More
VOTE
Hello Trupti Terse, did you try comparing oxygen plasma and acid cleaning ? Which one was good for you?
Hello Trupti Terse, did you try comparing oxygen plasma and acid cleaning ? Which one was good for you?
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Hello Prof Walter J Dressick and all,
I just wanted to know that what happened if the water is 2Mega-ohm deionized and after cleaning the glass with Dressick's protocol , is it right to do silanization with ethanol solution. Can you tell me the further protocol for silanization with ethanol? @Walter J Dressick
Hello Prof Walter J Dressick and all,
I just wanted to know that what happened if the water is 2Mega-ohm deionized and after cleaning the glass with Dressick's protocol , is it right to do silanization with ethanol solution. Can you tell me the further protocol for silanization with ethanol? @Walter J Dressick
More
VOTE
If this discussion is active still, could someone let me know how we may confirm that the monolayer of APTES on the glass slide is uniform. In the papers below, (1) Nath, Nidhi, and Ashutosh Chilkoti. "A colorimetric gold nanoparticle sensor to interrogate biomolecular interactions in real time on a surface." Analytical chemistry 74.3 (2002): 504-509. and (2) Nath, Nidhi, and Ashutosh Chilkoti. "Label-free biosensing by surface plasmon resonance of nanoparticles on glass: optimization of nanoparticle size." Analytical Chemistry 76.18 (2004): 5370-5378. it has been mentioned that the glass slides must be sonicated 5 times in ethanol. However, every time, I see a white-colored precipitate on the glass slide after the 3 hr, 120 deg C drying step. While following this step, I see gold nanoparticle aggregates on the surface, even if I sonicate the colloidal sample prior to deposition. It must be noted that I used microscope glass slide instead of cover glass slide. I would like to know why "cover glass slide" is preferred to "microscope glass slide" for chemisorption of gold nanoparticles?
If this discussion is active still, could someone let me know how we may confirm that the monolayer of APTES on the glass slide is uniform. In the papers below, (1) Nath, Nidhi, and Ashutosh Chilkoti. "A colorimetric gold nanoparticle sensor to interrogate biomolecular interactions in real time on a surface." Analytical chemistry 74.3 (2002): 504-509. and (2) Nath, Nidhi, and Ashutosh Chilkoti. "Label-free biosensing by surface plasmon resonance of nanoparticles on glass: optimization of nanoparticle size." Analytical Chemistry 76.18 (2004): 5370-5378. it has been mentioned that the glass slides must be sonicated 5 times in ethanol. However, every time, I see a white-colored precipitate on the glass slide after the 3 hr, 120 deg C drying step. While following this step, I see gold nanoparticle aggregates on the surface, even if I sonicate the colloidal sample prior to deposition. It must be noted that I used microscope glass slide instead of cover glass slide. I would like to know why "cover glass slide" is preferred to "microscope glass slide" for chemisorption of gold nanoparticles?
More
VOTE
I have been making self-assembled organosiloxane monolayers for 25 years. The cleaning method I use is: (1) Soak glass slides in a solution comprising one volume of concentrated HCl and one volume of methanol for at least 30 minutes (longer times are OK) to degrease the surface. (2) Rinse the slides THOROUGHLY (at least 4 times) with 18.2 Megaohm-cm deionized water. (3) Soak the slides in concentrated sulfuric acid for at least 30 minutes (longer times are OK). (4) Rinse the slides thoroughly (at least 4 times) in 18.2 Megaohm-cm deionized water. (5) Place the clean slides in gently boiling 18.2 Megaohm-cm deionized water for 30 minutes. (6) Remove the slides from the gently boiling water and dry them thoroughly using filtered nitrogen gas from liquid nitrogen boil-off. (7) Place slides in the organosilane treatment solution. This method has produced reliably clean slides for monolayer deposition for me. It avoids the use of dangerous piranha solutions as cleaning agents. The rinse step in step (2) is very important. If all the HCl-methanol is not removed, the sulfuric acid will react with it to leave a deposit on the glass surface. Do not use compressed nitrogen gas from tanks in step (6) because it may contain trace oil from pumps used to fill the tank that would deposit on the clean glass. The cleaning process described is thought to maximize the surface Si-OH concentration for monolayer deposition.
I have been making self-assembled organosiloxane monolayers for 25 years. The cleaning method I use is: (1) Soak glass slides in a solution comprising one volume of concentrated HCl and one volume of methanol for at least 30 minutes (longer times are OK) to degrease the surface. (2) Rinse the slides THOROUGHLY (at least 4 times) with 18.2 Megaohm-cm deionized water. (3) Soak the slides in concentrated sulfuric acid for at least 30 minutes (longer times are OK). (4) Rinse the slides thoroughly (at least 4 times) in 18.2 Megaohm-cm deionized water. (5) Place the clean slides in gently boiling 18.2 Megaohm-cm deionized water for 30 minutes. (6) Remove the slides from the gently boiling water and dry them thoroughly using filtered nitrogen gas from liquid nitrogen boil-off. (7) Place slides in the organosilane treatment solution. This method has produced reliably clean slides for monolayer deposition for me. It avoids the use of dangerous piranha solutions as cleaning agents. The rinse step in step (2) is very important. If all the HCl-methanol is not removed, the sulfuric acid will react with it to leave a deposit on the glass surface. Do not use compressed nitrogen gas from tanks in step (6) because it may contain trace oil from pumps used to fill the tank that would deposit on the clean glass. The cleaning process described is thought to maximize the surface Si-OH concentration for monolayer deposition.
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VOTE
Does concentrated nitric acid work equally well in place of conc. sulfuric acid here? Also, has anyone tried more dilute (1M) acid at longer intervals for cleaning/activation?
Does concentrated nitric acid work equally well in place of conc. sulfuric acid here? Also, has anyone tried more dilute (1M) acid at longer intervals for cleaning/activation?
More
VOTE
Dear Dr. Vu:
Mix 1 volume of concentrated (12 M) HCl and one volume of pure methanol- add the HCl carefully with stirring to the methanol. For the sulfuric acid, use concentrated sulfuric acid directly. Rinse substrates well with deionized water after removal from each of these acid solutions.
Dear Dr. Vu:
Mix 1 volume of concentrated (12 M) HCl and one volume of pure methanol- add the HCl carefully with stirring to the methanol. For the sulfuric acid, use concentrated sulfuric acid directly. Rinse substrates well with deionized water after removal from each of these acid solutions.
More
VOTE
Add the methanol to a beaker and initiate stirring. Slowly pour the HCl down a glass stir rod into the stirring methanol (i.e., add the HCl slowly to the stirred methanol. Do NOT add methanol to a volume of HCl to avoid local superheating and splashing). Work in a well-ventilated fume hood. Wear safety eye goggles, a lab coat, and gloves. Consult the MSDS forms for methanol and HCl for any other hazards and safety information BEFORE beginning.
Add the methanol to a beaker and initiate stirring. Slowly pour the HCl down a glass stir rod into the stirring methanol (i.e., add the HCl slowly to the stirred methanol. Do NOT add methanol to a volume of HCl to avoid local superheating and splashing). Work in a well-ventilated fume hood. Wear safety eye goggles, a lab coat, and gloves. Consult the MSDS forms for methanol and HCl for any other hazards and safety information BEFORE beginning.
More
VOTE
Hello Professor Walter J Dressick and others,
It would be nice of you if I can have your opinion regarding my experimental silanization process. I am using the Piranha cleaned glass substrates (contact angle 5°, after Piranha cleaning) for the silanization process. The silane I am using is N-trimethoxysilylpropyl. I add 1 mL of silane into 50 mL of de-ionized water and heat the solution with magnetic stirring at 80°C for 30 mins. After that I rinse it with extensive water for 30 mins and gave supersonic bath treatment for 30 mins. and dried under vacuum for 1 h. But unfortunately, the glass substrates were not rendered hydrophobic. I observed the contact angle of only 30° after silane treatment.
Can any body help/suggest me in this regard?
Thank you and BR,
Hello Professor Walter J Dressick and others,
It would be nice of you if I can have your opinion regarding my experimental silanization process. I am using the Piranha cleaned glass substrates (contact angle 5°, after Piranha cleaning) for the silanization process. The silane I am using is N-trimethoxysilylpropyl. I add 1 mL of silane into 50 mL of de-ionized water and heat the solution with magnetic stirring at 80°C for 30 mins. After that I rinse it with extensive water for 30 mins and gave supersonic bath treatment for 30 mins. and dried under vacuum for 1 h. But unfortunately, the glass substrates were not rendered hydrophobic. I observed the contact angle of only 30° after silane treatment.
Can any body help/suggest me in this regard?
Thank you and BR,
More
VOTE
There are many ways to clean glass for such experiments.
People generally saturated KOH, piranna etch or NH4OH, H2O2 and HCL.
KOH treatment and plasma cleaning renders glass hydrophilic
we compared different chemical treatments on glass at nanometer scale here using Atomic force microscopy
Article Glass is a Viable Substrate for Precision Force Microscopy o...
There are many ways to clean glass for such experiments.
People generally saturated KOH, piranna etch or NH4OH, H2O2 and HCL.
KOH treatment and plasma cleaning renders glass hydrophilic
we compared different chemical treatments on glass at nanometer scale here using Atomic force microscopy
Article Glass is a Viable Substrate for Precision Force Microscopy o...
More
VOTE
I don't know what "opac" layers are. After the RCA treatment, the glass is clear and completely wetted by water. I have not used an acrylate silane for chemisorption. If you see a film after chemisorption, it probably means you have a multilayer formed by silanol and/or vinyl group polymerization. In that case, you need to experiment and change your chemisorption conditions to get a uniform monolayer film (if that is what you are trying to make).
I don't know what "opac" layers are. After the RCA treatment, the glass is clear and completely wetted by water. I have not used an acrylate silane for chemisorption. If you see a film after chemisorption, it probably means you have a multilayer formed by silanol and/or vinyl group polymerization. In that case, you need to experiment and change your chemisorption conditions to get a uniform monolayer film (if that is what you are trying to make).
More
VOTE