HPSTM Products Series
Vapor Sublimation Trap
OPERATION AND
MAINTENANCE MANUAL
HPSTM Products Series Trap
Vapor Sublimation Trap
September 1997
PART #WCTRAP-MAN REV. A
Vapor Sublimation Trap
Part # WCTRAP-XXX-XXX-X-XXX
Serial # __ __ __ __ __ __
Please fill in these numbers and have
them readily available when calling for
service or additional information.
(The part number can be found on your
packing slip, and both the part number
and serial number are located on the
bottom side of the housing.)
For more information or literature, contact:
MKS Instruments Inc., HPSTM Products, Inc.
5330 Sterling Drive
Boulder, CO 80301 USA
Phone:
303-449-9861
800-345-1967
FAX:
303-442-6880
© 1997 by MKS Instruments Inc., HPSTM Products, Inc. All rights reserved.
Viton is a registered trademark of E.I. du Pontde Nemours & Co.
VacuComp is a trademark of MKS Instruments, HPSTM Products, Inc
Vapor Sublimation Trap
Table of Contents
Table of Contents
Package Contents ..................................................................... 1
Symbols Used in this Manual .................................................... 1
Safety Information...................................................................... 2
Symbols Used in this Manual (English) ..............................................
Symboles utilisés dans ce manuel (Français) .....................................
In dieser Betriebsanleitung vorkommende Symbole (Deutsch) ...........
Símbolos Usados en el Manual (Español) ..........................................
Definition of Symbols Found on the Unit (English) ..............................
Définition des symboles apparaissant sur l’appareil (Français) ...........
2
2
3
3
4
4
Symbol Definitions .................................................................... 4
Símbolos que Aparecen en la Unidad (Español) ................................. 4
Definitionen der am Gerät angebrachten Symbole (Deutsch) .............. 4
Safety Precautions .................................................................... 5
Chemical Handling .............................................................................. 5
Ammonium Chloride .................................................................................................. 5
Aluminum Chloride ..................................................................................................... 5
Feature and Control Locations .................................................. 6
Specifications ............................................................................ 8
Typical Applications for the Vapor Sublimation Trap .................. 9
About the HPSTM Vapor Sublimation Trap ................................ 10
Installing the Vapor Sublimation Trap ...................................... 11
Orienting the Trap ............................................................................... 11
Locating the Trap ................................................................................11
Wet Pump .......................................................................................... 11
Dry Pump ........................................................................................... 12
Using Cooling Water ........................................................................... 13
Maintaining the Vapor Sublimation Trap .................................. 14
Cleaning the Trap ................................................................................14
NH4Cl ................................................................................................. 14
AlCl3 ..................................................................................................14
Drying the Trap ...................................................................................15
Waste Management ........................................................................... 15
Accessories / Part Replacement ............................................. 16
Product Warranty ..................................................................... 17
Notes ....................................................................................... 18
Vapor Sublimation Trap
Appendix A: ......................... A.1
Vapor Pressure Curves ...... A.1
NH4Cl
AlCl3
A.1
A.2
Vapor Sublimation Trap
Package Contents
Before unpacking your Vapor Sublimation Trap, check all surfaces of the
packing material for shipping damage.
Please be sure that your Vapor Trap package contains these items:
t
1 Trap unit
t
1 HPS™ Vapor Sublimation Trap User's Manual
Inspect the Trap for visible evidence of damage. If it has been damaged in
shipping, notify the carrier immediately. Keep all shipping materials and
packaging for claim verification. Do not return the product to HPSTM.
If any items are missing from the package, call HPSTM
Customer Service at 1-303-449-9861 or 1-800-345-1967.
Symbols Used in this Manual
The first two symbols, that may be located on your HPSTM, Vapor
Simulation Trap identify critical safety concerns. They are used
throughout this manual to further define the safety concerns associated
with the product.
The last two symbols identify other information in this manual that is
essential or useful in achieving optimal performance from the HPSTM,
Vapor Simulation Trap.
Vapor Sublimation Trap
1
Safety Information
Symbols Used in this
Manual
(English)
Definitions of CAUTION and
NOTE messages used throughout
the manual.
22
Symboles utilisés dans
ce manuel
(Français)
Définition des indications
ATTENTION et REMARQUE
utilisées dans ce manuel.
CAUTION: Refer to
accompanying documents.
ISO 3864, No. B.3.1
ATTENTION: Se reporter à la
documentation. ISO 3864, No. B.3.1
This sign denotes a hazard.
It calls attention to a
procedure, practice,
condition, or the like, which,
if not correctly performed or
adhered to, could result in
injury to personnel.
L’indication signale un danger
potentiel. Elle est destinée à attirer
l’attention sur une procédure, une
utilisation, une situation ou toute
autre chose présentant un risque de
blessure en cas d’exécution
incorrecte ou de non-respect des
consignes.
This sign denotes a hazard.
It calls attention to an
operating procedure,
practice, or the like, which, if
not correctly performed or
adhered to, could result in
damage to or destruction of
all or part of the product.
L’indication signale un danger
potentiel. Elle est destinée à attirer
l’attention sur une procédure, une
utilisation, une situation ou toute
autre chose présentant un risque
d’endommagement ou de dégât
d’une partie ou de la totalité de
l’appareil en cas d’exécution
incorrecte ou de non-respect des
consignes.
This sign denotes important
information. It calls attention
to a procedure, practice,
condition, or the like, which
is essential to highlight.
L’indication REMARQUE signale
des informations importantes. Elle
est destinée à attirer l’attention sur
une procédure, une utilisation, une
situation ou toute autre chose
présentant un intérêt particulier.
Vapor Sublimation Trap
In dieser
Betriebsanleitung
vorkommende
Symbole (Deutsch)
Símbolos Usados en el
Manual
(Español)
Definiton der mit VORICHT! und
HINWEIS überschriebenen
Abschnitte in dieser
Betriebsanleitung.
Definiciones de los mensajes de
PRECAUCIÓN y OBSERVACIÓN
usados en el manual.
VORSICHT! Bitte Begleitdokumente
lesen! ISO 3864, Nr. B.3.1
PRECAUCIÓN: Consultar los documentos adjuntos. ISO 3864, N.° B.3.1
Das Symbol VORSICHT! weist auf
eine Gefahrenquelle hin. Es macht
auf einen Arbeitsablauf, eine
Arbeitsweise, einen Zustand oder
eine sonstige Gegebenheit
aufmerksam, deren unsachgemäße
Ausführung bzw. Ungenügende
Berücksichtigung zu
Körperverletzung führen kann.
Esto símbolo indica un riesgo. Pone
de relieve un procedimiento,
práctica, condición, etc., que, de no
realizarse u observarse
correctamente, podría causar
lesiones a los empleados.
Das Symbol VORSICHT! weist auf
eine Gefahrenquelle hin. Es macht
auf einen Bedienungsablauf, eine
Arbeitsweise oder eine sonstige
Gegebenheit aufmerksam, deren
unsachgemäße Ausführung bzw.
Ungenügende Berücksichtigung zu
einer Beschädigung oder
Zerstörung des Produkts oder von
Teilen des Produkts führen kann.
Esto símbolo indica un riesgo.
Pone de relieve un procedimiento,
práctica, etc., de tipo operativo
que, de no realizarse u observarse
correctamente, podría causar
desperfectos al instrumento, o
llegar incluso a causar su
destrucción total o parcial.
Das Symbol HINWEIS weist auf
eine wichtige Mitteilung hin, die
auf einen Arbeitsablauf, eine
Arbeitsweise, einen Zustand oder
eine sonstige Gegebenheit von
besonderer Wichtigkeit
aufmerksam macht.
Esto símbolo indica información
de importancia. Pone de relieve
un procedimiento, práctica,
condición, etc., cuyo
conocimiento resulta esencial.
Vapor Sublimation Trap
3
Symbol Definitions
Definition of
Symbols Found
on the Unit
(English)
Definitionen der am
Gerät angebrachten
Symbole (Deutsch)
Caution
refer to accompanying documents
ISO 3864, No. B.3.1
Vorsicht!
Bitte Begleitdokumente
lesen!
ISO 3864, Nr. B.3.1
Caution
hot surface
IEC 417, No. 5041
Vorsicht!
Heiße Fläche!
IEC 417, Nr. 5041
Frame or Chassis
IEC 417, No. 5020
Rahmen oder Chassis
IEC 417, Nr. 5020
Class II Equipment
IEC 417, No. 5172-a
Geräteklasse II
IEC 417, Nr. 5172-a
Définition des symboles Símbolos que Aparecen
apparaissant sur
en la Unidad (Español)
l’appareil (Français)
Attention
se reporter à la documentation
ISO 3864, No. B.3.1
Precaución
Consultar los documentos
adjuntos
ISO 3864, N.° B.3.1
Attention
surface brûlante
IEC 417, No. 5041
Precaución
Superficie caliente
IEC 417, N.° 5041
Masse, Châssis
IEC 417, No. 5020
Caja o chasis
IEC 417, N.° 5020
Matériel de la Classe II
IEC 417, No. 5172-a
Equipo de clase II
IEC 417, N.° 5172-a
44
Vapor Sublimation Trap
Safety Precautions
The following general safety precautions must be observed during all
phases of operation of this product. Failure to comply with these
precautions or with specific warnings elsewhere in this manual violates
safety standards of intended use and may impair the protection provided by
the equipment. HPS Division of MKS Instruments, Inc. assumes no liability
for the customer’s failure to comply with these requirements.
Chemical Handling
Refer to your Material Safety Data Sheets (MSDS).
Ammonium Chloride
NH4Cl may be harmful by inhalation, ingestion, or skin
absorption. Causes eye and skin irritation.
Do not breathe its dust.
Avoid contact with eyes, skin, and clothing. When working with NH4Cl, be
sure to wear a NIOSH/MSHA approved respirator, chemical resistant
gloves, safety goggles, and other protective clothing. Wash up thoroughly
after handling the chemical.
NH4Cl is corrosive and soluble in water.
Aluminum Chloride
AlCl3 is highly toxic. It may be harmful by inhalation, ingestion,
or skin absorption.
Do not breathe the vapors and use only in a chemical fume hood.
Avoid contact with eyes, skin, and clothing. When working with AlCl3, be
sure to wear a NIOSH/MSHA approved respirator, chemical resistant
gloves, safety goggles, and other protective clothing. Wash up thoroughly
after handling the chemical.
AlCl3 is corrosive and reacts violently with water.
Vapor Sublimation Trap
5
Feature and Control Locations
x
x
y
NW 50 Angle Trap
y
NW 50 Offset, Inline Trap
x
x
y
NW 80 Angle Trap
y
NW 80 Off-Set, Inline Trap
66
Vapor Sublimation Trap
x
y
x
NW 100 Angle Trap
y
NW 100 Off-Set, Inline Trap
DIMENSIONS
IN.
(MM)
INLINE
NW 50
NW 80
NW 100
ANGLE
NW 50
NW 80
NW 100
6" BODY
8"BODY
X
Y
X
9.5
10.5
9.2
12.3
(241)
(267)
(234)
(312)
Y
8.0
9.3
7.8
11.0
(203)
(236)
(198)
(279)
7.3
9.3
7.0
11.0
(185)
(236)
(178)
(279)
X
Y
X
Y
7.0
7.8
6.7
9.5
(178)
(198)
(170)
(241)
5.3
6.0
5.0
7.8
(135)
(152)
(127)
(198)
5.0
5.0
4.3
6.8
(127)
(127)
(109)
(173)
Vapor Sublimation Trap
7
Specifications
Body Diameter
6 or 8 in.
Capacity
6-inch
3.0 lb (1.4 kg) NH4Cl
4.5 lb (2.0 kg) AlCl3
8-inch
10.0 lb (4.5 kg) NH4Cl
15.0 lb (6.8 kg) AlCl3
Efficiency
> 99 %
Flow Conductance
(Viscous Flow Region)
C (L/sec) = 20.74p
p – pressure in mTorr
Pressure Drop Across Trap
(Viscous Flow Region)
p (mTorr) = 812 Q/p2
Q – gas flow rate in sccm
p – pressure in mTorr
Cooling Water Flow Rate
> 6 gal/hr (400 mL/min)
Cooling Water Temperature
< 86°F (30°C), lower is better
Materials
304 and 316 series stainless steel,
elastomer seal
Flanges/Interface
MF 100, MF 80
KF 100, KF 80, KF 50
Reducers are required and available
for MF 63 and KF 40 pump lines
Typical Dry Weight with MF
Flanges
6-inch
16.5 lb (7.5 kg)
8-inch
28.0 lb (12.7 kg)
Design and/or specifications subject to change without notice.
88
Vapor Sublimation Trap
Typical Applications for the
Vapor Sublimation Trap
vv
Collect ammonium chloride (NH4Cl) in a silicon nitride CVD system
vv
Collect aluminum chloride (AlCl3) in an aluminum etching system
vv
Trap condensable vapors that begin to solidify above
ambient temperature
Vapor Sublimation Trap
9
About the HPSTM
Vapor Sublimation Trap
CHEMICAL REACTION PROCESSES, such as Chemical Vapor Deposition (CVD),
are carried out under high temperature and vacuum conditions such that a
high reaction rate can be reached and particulate contamination lessened.
Ammonium chloride (NH4Cl) by-product from silicon nitride
CVD and aluminum chloride (AlCl3) by-product
from aluminum etching solidify
above ambient temperature.
Resulting clogged pump lines
and contaminated systems
require frequent maintenance.
The HPS™ Vapor
Sublimation Trap collects
these condensable vapors,
significantly reducing
maintenance and increasing
throughput. Its efficiency
rating of more than 99% and
high capacity ensure less
down time and higher
product yield, making it
especially desirable to the
semiconductor industry.
The Trap is designed with
two stages — the first for high
capacity, the second for
attaining high trapping
efficiency. The first stage, at
the entrance of the Trap, has a
higher volume for collecting
condensable by-product than
comparable traps. In fact, its
capacity is approximately 5 to 10
times greater than other traps of
the same class.
Several perforated stainless steel cones
are placed in the second stage to maximize
the heat transfer between the gas and cooling
surface while maintaining the necessary high flow
conductance. This is a final “polish” of the gas flow.
10
10
Vapor Sublimation Trap
Installing the
Vapor Sublimation Trap
Orienting the Trap
The orientation of the Trap has a negligible effect on the performance of the
Trap as the condensed ammonium chloride and aluminum chloride are very
hard, dense materials.
The Vapor Trap must be installed in the correct flow direction,
indicated by the arrow sign on the Trap body, to attain its
highest capacity and efficiency.
Locating the Trap
Figure 1 at the bottom and figure 2 on the next page show Trap installation
suggestions for a wet pump and a dry pump, respectively. Shaded areas
represent heated lines or components, while unshaded areas represent
unheated or cold lines or components.
Wet Pump
As shown in figure 1A, when the Trap is installed next to a wet pump and
not in a clean room, replacement of the Trap is greatly simplified.
Figure 1B shows the Trap located just downstream of a heated isolation
valve. This locale option shortens the length of heated line.
In any case, always install the Trap upstream of a wet pump.
A
B
Figure 1: Installation options with a wet pump
Vapor Sublimation Trap
11
A
B
C
D
Figure 2: Installation options with a dry pump.
Dry Pump
Though a trap is not required with a dry pump (figure 2A), one should be
used to improve the overall performance of your system and process yield.
If the Trap is installed downstream of the pump, as in figure 2B, the Scrubber
load is reduced dramatically and heated lines post-Trap are not needed since
most of the condensable vapors have been collected in the Trap.
In figures 2C and 2D, the Trap is installed upstream of the pump to prevent
solidified vapors from clogging or damaging it. This option also reduces the
amount of ballast nitrogen dramatically, thus improving both the
performance and lifetime of the dry pump.
With a Trap, you can use an unheated roots blower to achieve higher
pumping speed and lower the ultimate pressure in a CVD system.
General rules for locating the Trap are:
v
v
v
12
12
Apply heat to the pump line between the reaction chamber and
the Trap,
Place a heated isolation valve between the reaction chamber and
the Trap, and
Install the Trap more than 3 feet away from the exit of the
reaction chamber.
Vapor Sublimation Trap
Using Cooling Water
Cooling water should be provided to attain high efficiency from the Trap.
House water or refrigerated water is acceptable. The water flow rate should
be kept at approximately 6 gallons per hour or higher. The temperature of
the cooling water should be less than 30°C, a lower water temperature is
preferred.
Vapor pressure curves for both ammonium chloride and aluminum chloride
are shown in Appendix A. These curves show at what temperatures heated
lines located before the Trap operate most efficiently as a function of
pressure, as well as the partial pressure of the condensable vapor leaving
the Trap.
Vapor Sublimation Trap
13
Maintaining the
Vapor Sublimation Trap
Since the Vapor Trap is used to collect such by-products as solidified
ammonium chloride (NH4Cl) or aluminum chloride (AlCl3), the conductance
of the Trap will decrease after a period of operation. Eventually, the Trap
will limit gas flow rate due to the condensed solid, and periodical cleaning in
a water bath with follow-up baking is necessary.
Cleaning the Trap
NH4Cl
Since NH 4Cl is soluble in water, clean the Trap in a water bath.
Mechanical cleaning is not recommended since solidified NH4 Cl is a
very strong, harsh material.
Do not attempt to separate internal from trap body prior to
cleaning. Failing to do so may result in significant damage
to the trap.
1
Insert the Trap into a fresh, circulating warm water bath. Since the
solubility of NH4Cl in water is a function of temperature, cleaning
time will be shortened if warm water is used. Lukewarm water
(<60°C) is recommended.
2
Continuously circulate the water bath during the cleaning process to
lower the acidity of the solution for minimal corrosion. A fresh water
pressurized rinse is preferred.
Do not use hot water. HCl acid may be generated during the
dissolving process prematurely corroding the Trap body.
3
When removing internasal from body, be sure to pull internal
out axially do not spin or twist the internal, or damage to the
coils could result.
AlCl3
If collecting AlCl3 in the Trap, cold water (<30°C) should be used to clean it
since the solubility for AlCl3 is much higher than for NH4Cl. High levels of
HCl acid will be generated if hot water is used.
AlCl3 reacts violently with water. Special safety procedures
should be followed during the cleaning process.
14
14
Vapor Sublimation Trap
Drying the Trap
Place the Trap in an oven to dry for about 2 hours after cleaning in the
water bath. Set the oven temperature to less than 120°C. A higher
temperature may vaporize the water concealed in the cooling coils by the
quick-release couplings.
Since large amounts of by-product are collected in the Trap, it may take
several hours to complete the whole cleaning and drying process.
It is highly recommended that a spare Trap be available and
used to replace the other during cleaning to minimize
downtime. Water vapor contamination, due to environment
exposure, will also be reduced.
Waste Management
Please consult with your local waste management authorities for proper
disposal of hazardous chemical waste.
Vapor Sublimation Trap
15
Accessories / Part Replacement
Part #
Replacement Internal
6-inch Body
8-inch Body
100004954
100009608
Bonnet Flange Seal
For 6-inch Body
Viton®
Silicone
100003597
100004790
For 8-inch Body
Viton®
Silicone
100762020
100009637
1
Self-Sealing, Quick-Release H2O Fitting
Straight, Qty 2
90° Elbow, Qty 2
100004980
100004981
Please call HPSTM' Customer Service Department at 1-303-449-9861 or
1-800-345-1967 to order any of these accessories or to receive catalogs for
other HPSTM Products.
16
16
Vapor Sublimation Trap
Product Warranty
Extent of the Warranty
MKS Instruments, Inc., warrants the HPS TM Vapor Sublimation Trap and its accessories to be free from
defects in materials and workmanship for one (1) year from the date of shipment by HPSTM or authorized
representative to the original purchaser (PURCHASER). Any product or parts of the product repaired or
replaced by HPSTM under this warranty are warranted only for the remaining unexpired part of its one (1)
year original warranty period. After expiration of the applicable warranty period, the PURCHASER shall be
charged HPSTM’ current prices for parts and labor, plus any transportation for any repairs or replacement.
ALL EXPRESS AND IMPLIED WARRANTIES, INCLUDING THE IMPLIED WARRANTIES OF
MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE, ARE LIMITED TO THE WARRANTY
PERIOD. NO WARRANTIES, EXPRESS OR IMPLIED, WILL APPLY AFTER THIS PERIOD.
Warranty Service
The obligations of HPSTM under this warranty shall be at its option: (1) to repair, replace, or adjust the
product so that it meets applicable product specifications published by HPSTM or (2) to refund the purchase
price.
What Is Not Covered
The product is subject to above terms only if located in the country of the seller from whom the product
was purchased. The above warranties do not apply to:
I. Damages or malfunctions due to failure to provide reasonable and necessary maintenance in
accordance with HPSTM operating instructions.
II. Damages or malfunctions due to chemical or electrolytic influences or use of the product in
working environments outside the specification.
III. Fuses and all expendable items which by their nature or limited lifetime may not function for a year. If
such items fail to give reasonable service for a reasonable period of time within the warranty period
of the product; they will, at the option of HPSTM, be repaired or replaced.
IV. Defects or damages caused by modifications and repairs effected by the original PURCHASER or
third parties not authorized in the manual.
Condition of Returned Products
HPSTM will not accept for repair, replacement, or credit any product which is asserted to be defective by
the PURCHASER, or any product for which paid or unpaid service is desired, if the product is contaminated
with potentially corrosive, reactive, harmful, or radioactive materials, gases, or chemicals.
When products are used with toxic chemicals, or in an atmosphere that is dangerous to the health of
humans, or is environmentally unsafe, it is the responsibility of the PURCHASER to have the product
cleaned by an independent agency skilled and approved in the handling and cleaning of contaminated
materials before the product will be accepted by HPSTM for repair and/or replacement.
In the course of implementing this policy, HPSTM Customer Service Personnel may inquire of the
PURCHASER whether the product has been contaminated with or exposed to potentially corrosive,
reactive, harmful, or radioactive materials, gases, or chemicals when the PURCHASER requests a return
authorization. Notwithstanding such inquiries, it is the responsibility of the PURCHASER to ensure that no
products are returned to HPSTM which have been contaminated in the aforementioned manner.
Other Rights and Remedies
I. These remedies are exclusive. HPSTM SHALL NOT BE LIABLE FOR CONSEQUENTIAL DAMAGES,
FOR ANTICIPATED OR LOST PROFITS, INCIDENTAL DAMAGES OR LOSS OF TIME, OR OTHER
LOSSES INCURRED BY THE PURCHASER OR BY ANY THIRD PARTY IN CONNECTION WITH
THE PRODUCT COVERED BY THIS WARRANTY, OR OTHERWISE. Some states do not allow
exclusion or limitation of incidental or consequential damage or do not allow the limitation on how
long an implied warranty lasts. If such laws apply, the limitations or exclusions expressed herein
may not apply to PURCHASER.
II. Unless otherwise explicitly agreed in writing, it is understood that these are the only written
warranties given by HPSTM. Any statements made by any persons, including representatives of
HPSTM, which are inconsistent or in conflict with the terms of the warranty shall not be binding on
HPSTM unless reduced to writing and approved by an authorized officer of HPSTM.
III. This warranty gives PURCHASER specific legal rights, and PURCHASER may also have other rights
which vary from state to state.
IV. For HPSTM products sold outside of the U.S., contact your MKS representative for warranty
information and service.
Warranty Performance
To obtain warranty satisfaction, contact the following: MKS Instruments Inc., HPSTM Products, Inc., 5330
Sterling Drive, Boulder, CO 80301, USA, at phone number (303) 449-9861. You may be required to present
proof of original purchase.
Vapor Sublimation Trap
17
Notes
18
18
Vapor Sublimation Trap
Vapor Sublimation Trap
19
Appendix A:
Vapor Pressure Curves
NH4Cl
103
102
Solid Phase
101
Pressure
(Torr)
100
Vapor Phase
10-1
10-2
10-3
10-4
10-5
0
50
100
150
200
250
300
350
Temperature
(°C)
Vapor Sublimation Trap
A.1
AlCl3
103
102
Solid Phase
101
Pressure
(Torr)
100
10-1
Vapor Phase
10-2
10-3
10-4
10-5
0
A.2
50
Vapor Sublimation Trap
100
Temperature
(°C)
150
200