General Purpose Wet Bench
wbgeneral
Operating Instructions
The wbgeneral wet bench is for wet, non-solvent processing of standard and non-standard materials. Such materials include wafer pieces or substrates with gold or other non-standard films. Non-standard processing includes KOH etching of silicon and etching of non-standard substrates such as glass. There are no automated wafer processing modules at this station; all processing is done manually in station-dedicated or labuser-provided labware (beakers, dishes, etc.) With appropriate, dedicated quartzware, KOH cleanup can be done to decontaminate wafer for later processing in CMOS-compatible equipment. The station contains one hot plate and a constant temperature circulating bath for heating solutions in beakers. The station also contains a sink for rinsing, and an aspirator and HF drain for disposal of common waste. For additional process info, see section 9.
Substrates may be of most any type, size, shape and any material, subject to the constraints in the Materials Allowed section (1.3). GaAs, however, is not allowed for processing here.
The wbgeneral appears in all three equipment groups (clean, semiclean, and gold) as part of the general-purpose wet benches tool set. Processing may require dedicated labware (see section 4.1.2). Any labware at the wbgeneral station is considered gold-contaminated. For more details, consult the Materials Allowed section of the wbgeneral web page.
No solvents are allowed at this bench (solvent processing must be done at one of the solvent benches.) SNF standard etchants (consult the Materials List on the SNF website for acceptable chemicals) are allowed at this bench, for standard processing only. Consult staff if your work requires non-standard processing conditions (such as elevated temperatures, unusually extended process times, or mixing of chemicals), even if standard SNF etchants and chemicals are to be used.
The wbgeneral station has the following facilities: HF acid waste drain (awhf-f13), acid waste neutralization drain (awn-f15), deionized water (dih2o-f9), scrubber exhaust (exhsc-f16), house nitrogen (hn2-f1) and industrial water (iw-f12).
This is a Santa Clara Plastics brand wet bench. It is equipped with one heater module and a constant temperature bath, all used for heating solutions in beakers or other containers. These modules have controllers mounted in the upper panel. There is a separate, covered, HF disposal module which drains into the HF waste collection system. The aspirator and the rinse sink both drain into the acid waste neutralization system. The wet bench plenum, over which all the modules sit, collects runoff from the benchtop and drains into the acid waste neutralization system. The wet bench also contains an N2 gun and a DI water hand sprayer.
Because many commonly used etch processes are quite long yet may not require the operator to be present at all times (for example, KOH etching all the way through silicon), the wbgeneral station is set up to allow two users at once and, thus, has two Coral names ( wbgen-hpr, and wbgen-ctb.)
Any of the SNF-standard, non-solvent etchants may be in use at any time at this bench. Any non-SNF-approved etchants must undergo safety and contamination review by the SpecMat team (consult the Materials portion of the SNF website for the specific procedures.) Because this is a shared bench, you must read the Material Safety Data Sheets and be aware of the hazards, not only of the chemicals you are using, but also for chemicals that are commonly used here (see below and section 9) which may be in use by others. Because mixing and pouring of chemicals into open containers are performed at this wet bench, users must be keenly aware of the potential handling hazards of these chemicals. Be aware that wbgeneral is an entirely manual station, without safety features of other wet benches to prevent chemical mixing, spills, or other potential problems. Above all, users must understand and practice safe chemical handling procedures for working at this station.
Some of the chemicals you might find at this bench are: Sulfuric acid, hydrogen peroxide, hydrogen chloride, KOH, and hydrofluoric acid (50:1 HF, 20:1 BOE, 6:1 BOE, 49% HF) and mixtures thereof. You must read the Material Safety Data Sheets for these chemicals and understand safe chemical handling procedures before working at this station.
The primary hazard classifications for some of the chemical mixtures which may be used at this bench are:
For 70% - 90% sulfuric/peroxide -
Corrosive, oxidizer, air/water reactive
For 50:1 HF, 10:1 HF, 20:1 BOE and 6:1 BOE - Corrosive, toxic
For PRX-127 or PRS-1000 - Flammable, mildly corrosive
For Hot phosphoric - Corrosive, oxidizer, air/water reactive
30% KOH - Corrosive
20% TMAH, Tetra Methyl Ammonium Hydroxide- Corrosive
Remember: because of fire/explosion risk, flammables should not be mixed with corrosives or oxidizers.
HF-based chemicals may cause serious, delayed tissue damage upon skin contact. The mechanism of action is the depletion of calcium from muscle and bone by free fluoride, which can readily pass through skin. If skin contact with HF-based chemicals is suspected, rinse the affected area thoroughly, and then immediately apply calcium gluconate gel to the affected area, following the SNF guidelines for first aid for HF exposure. HF-kits containing tubes of gel (along with instructions for use) are located in plastic bags at each wet station.
Input power is 208 volts AC, three phase at 30 amps. Only qualified personnel are allowed to work on the electrical parts of this system. If any electrical problems are seen with this system, press the EMERGENCY POWER OFF button, shut the system down on Coral, and contact Maintenance staff.
General process hazards involve handling of chemicals and materials which come into contact with chemical used at this station. Wet benches are potentially the most dangerous operations in the lab, this particular one more so than the other because processing is completely manual. Be sure you understand all hazards and proper handling procedures before working at this or any other wet bench.
The wbgeneral bench has NO safety interlocks to protect personnel from chemical and process hazards described above. So it is absolutely imperative that users must thoroughly understand the chemicals, materials and processes they are working with and their associated hazards.
The sink, aspirator, and plenum all drain into the general lab acid waste neutralization (AWN) system. These modules may be used only when the AWN is functioning. When there is a problem with the AWN, the yellow light (above wbgaas/wbnonmetal) will flash. When the AWN warning system is flashing, no processing at any of the acid/base wet benches is allowed.
Operators of this station must be able to demonstrate or describe the activities on this list:
Chemical safety knowledge:
Contamination control knowledge:
Process knowledge:
Equipment knowledge:
4.1.2 Cassettes and other Labware
Cassettes at wbgeneral do not have any markings; some have been cut in half for ease of use in beakers. Any cassettes with buttons or circular cutouts belong to other wet bench stations and so must not be used at wbgeneral because they will become contaminated. (Another note: please handle Teflon cassettes with care -- they cost about $250 each to replace.)
Labware found at wbgeneral is considered gold-contaminated; any substrates processed in this labware is considered gold-contaminated thereafter. You may use your own personally labeled, dedicated labware to prevent contamination of substrates. In order to be "clean" compatible, the labware must never have been in contact with solutions or materials containing alkali (Na, K, Li) or any metals. To be "semiclean", labware must never come into contact with alkali nor any non-standard metals (standard metals are acceptable.) Personal labware must be stored in personal storage space or will be considered contaminated. Dedicated "clean" (uncontaminated) labware must be made of either fused silica ("quartz") or electronics-grade Teflon. Standard Pyrex-brand glassware, which contains up to 5% sodium, is unacceptable as "clean" labware.
Labware must be compatible with the etchant to be used. Pyrex is not acceptable for HF or BOE etchants, although it is acceptable for sulfuric/peroxide ("piranha") cleans. Likewise, for quartz. Teflon is acceptable for any of the commonly used etchants, although should not be heated (heat is transferred poorly and Teflon will absorb etchant). Polypropylene is not acceptable for piranha (as it melts) although is acceptable for room-temperature HF or BOE etchants. In summary:
|
Labware material |
Piranha |
HF or BOE |
KOH/TMAH |
|
Pyrex |
OK |
Will etch |
OK |
|
Quartz |
OK |
Will etch |
OK |
|
Teflon |
OK |
OK |
Chemically OK |
|
Polypropylene |
Chemically OK |
OK |
Chemically OK |
For other etchants and material combinations, you may wish to consult SNF staff.
The control panel modules are, from left to right are:
4.2.1.1 3130 EPO. This controls power to the control panel, this controls power to the control panel. It contains the Emergency Off button (top) and the main power On/Off switch. When in use or under standby conditions, the main power should always be left on (the Coral system will automatically turn the power off, when completely disabled.)
4.2.1.3 Gooseneck/Aspirator. This controls water flow at the bench. The "Gooseneck" switch turns the tap in the rinse sink on and off. The "Aspirator" switch turns on the aspirator system, allowing the user to drain chemicals (see section 4.5.3 for procedures.) After three minutes, the aspirator will turn itself off; press the switch again to restart.
4.2.1.5 Hot Plate Controller. This controls the heating element on the hot plate.
4.2.1.6 Constant Temperature Bath. This controls heating of the constant temperature bath.
4.5.1 Labeling Containers with Blue "In-use Hazardous Chemical" Tags:
|
Antimony |
Arsenic |
Barium |
Beryllium |
|
Boron |
Cobalt |
Manganese |
Molybdenum |
|
Selenium |
Thallium |
Vanadium |
Cyanide |
|
Formaldehyde |
Gold |
Phenols |
Any chemicals on the Federal List of Acutely Hazardous Chemicals or the California List of Extremely Hazardous Chemicals must also be collected locally. When in doubt, check with the SNF staff.
Clean up your workspace. Ensure the benchtop is clean and dry. Turn off the heater/stirrers or constant temperature bath if you have used them; otherwise, leave them on (if someone else is using them). Leave the main power on. Disable the module you used (wbgen-hpr, or wbgen-ctb) on Coral. Be sure you are leaving the station in neat condition (see section 5.1).
5. ROUTINE MAINTENANCE AND CALIBRATION
Bench top and plenum should be thoroughly rinsed and drained. Main power should be shut off to the system.
The wbgaas wet bench may be used in much the same way as wbgeneral. However, priority at wbgaas is given to researchers with GaAs processes to run.
Background information on some of the processes which are commonly run at wbgeneral is given here. Detailed information and procedures for these and other processes commonly performed at wbgeneral are listed on the website at:
http://snf.stanford.edu/Equipment/wbgeneral/ProcessInfo.html
9.1 90% Sulfuric/Peroxide Photoresist Strip Piranha Clean
This solution consists of 90% concentrated sulfuric acid and 10% hydrogen peroxide and is heated to 120 +/- 10 degrees C. Sulfuric acid is about 95%-98% pure; the hydrogen peroxide in the lab is 30% in water. This combination is excellent for removing organics. The sulfuric acid converts organic compounds to elemental carbon (which is why the solution may darken temporarily when loaded with photoresist). The peroxide then oxidizes the carbon to carbon dioxide and water (which is why the solution boils and fumes, and eventually clears again.) When the piranha mixture has been around for a while or has been used extensively, the hydrogen peroxide all turns to water, which is a lousy oxidant in this system. So, additional hydrogen peroxide can be added on an as-needed basis to increase the active lifetime of the piranha. However, for the temperatures that we run, additional peroxide can help only so much before the acid becomes diluted and then needs to be changed. For regular usage levels in our lab, a change frequency of about once/week is generally sufficient.
9.2 4:1 Sulfuric/Peroxide Piranha Clean
This solution consists of 80% concentrated sulfuric acid and 20% hydrogen peroxide. The 4:1 piranha clean is run at 90 degrees C, which is lower than the standard process temperature for 90% clean for photoresist removal. At this station, this dip serves the same purpose as the first SC-1 step of the RCA standard clean process, in removing any trace organics.
There are several varieties of HF-based etchants, different in acid strength and in composition. HF-based etchants include the BOE etchants, Pad etch, and ammonium fluoride (NH4F). Before working with any HF-based etchant, read the information and the links provided in the Safety section about HF.
9.3.1 HF/Water Mixtures: 50:1 HF and 49% HF
SNF stocks two "straight HF" mixtures (which contain only HF and water): 50:1 HF and 49% HF.
Concentrated hydrofluoric acid is approximately 49% HF and 51% water. 50:1 HF is approximately 2% HF in water, about 25-fold less than 49%. Do not confuse these two (yes, this mistake has been made). The 49% HF bottles should have an eye-catching magenta-colored ty-rap around the neck of the bottle.
The etch rate of thermal oxide in 50:1 HF is generally nominal (about 50 angstroms/minute.) Because this acid is not buffered, the etch rate may vary with acid lifetime or usage. More detailed etch rate info is available on the Processes section of the SNF website.
9.3.2 Buffered Oxide Etchants: BOE
BOE is the acronym for "Buffered Oxide Etch", which is a mixture of ammonium fluoride, HF, and water. Ammonium fluoride is normally a solid with a low temperature of sublimation, but is very soluble in water (concentrated ammonium fluoride is approximately 40% by weight in water.) In the BOE etchants, the ammonium fluoride acts as a buffer, maintaining the pH of the solution which keeps the etch rate stable/constant over time. High concentrations of ammonium fluoride are used in BOE; in fact, the total fluoride ion content is nearly that of concentrated 49% HF, and so BOE etchants are considered to pose the same toxic hazards as 49% HF.
The temperature of BOE etchants is not controlled in SNF. Depending on the manufacturer, BOE acids may also have an added surfactant to help circumvent surface tension, which can prevent etching in small geometries or in areas with high aspect ratios. The exact formulations of BOE's are generally proprietary, but here is a general summary is below.
20:1 BOE is approximately 20 parts of 40% ammonium fluoride and 1 part of 49% HF. Thus, 20:1 BOE is approximately 38% NH4F, 2.5% HF, and 60% water. The etch rate of thermal oxide is approximately 300 angstroms/minute. More detailed etch rate info is available on the SNF website.
6:1 BOE is approximately 6 parts of 40% ammonium fluoride and 1 part of 49% HF. Thus, 6:1 BOE is approximately 34% NH4F, 7% HF, and 59% water. The etch rate of thermal oxide is approximately 900 angstroms/minute. More detailed etch rate info is on the SNF website.
Heated 30% KOH in water is used to etch silicon. 45% KOH can be found in the Chemicals passthrough and can be diluted to provide a 30% solution. Detailed procedures for KOH etching can be found in the processes link. KOH is a strong, corrosive base and should be handled with extreme care. Potassium is an extremely fast-diffusing alkali metal which will have disastrous effects on the performance of any electronic device should it come into contact with any wafers, wafer handling tools, or processing equipment in the "clean" or "semiclean" equipment groups. Be extremely careful about handling KOH and all the labware and wafers which come into contact with it. Be extremely conscientious about decontaminating your substrates if they are to be returned to "clean" or "semiclean" equipment.
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Stanford Nanofabrication Facility webmaster@snf.stanford.edu Last Modified 06/09/2008 |