HPS Products SeriesVapor Sublimation Trap 1 The first two symbols, that may be located on your...

HPSTM Products SeriesVapor Sublimation Trap

OPERATION ANDMAINTENANCE MANUAL

Vapor Sublimation Trap

HPSTM Products Series TrapVapor Sublimation Trap

September 1997PART #WCTRAP-MAN REV. A


Part # WCTRAP-XXX-XXX-X-XXX

Serial # __ __ __ __ __ __

Please fill in these numbers and havethem readily available when calling forservice or additional information.

(The part number can be found on yourpacking slip, and both the part numberand serial number are located on thebottom side of the housing.)

© 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

For more information or literature, contact:

MKS Instruments Inc., HPSTM Products, Inc.5330 Sterling DriveBoulder, CO 80301 USA

Phone: 303-449-9861800-345-1967

FAX: 303-442-6880


Table of Contents

Table of ContentsPackage Contents ..................................................................... 1Symbols Used in this Manual .................................................... 1Safety Information...................................................................... 2

Symbols Used in this Manual (English) .............................................. 2Symboles utilisés dans ce manuel (Français) ..................................... 2In dieser Betriebsanleitung vorkommende Symbole (Deutsch) ........... 3Símbolos Usados en el Manual (Español) .......................................... 3Definition of Symbols Found on the Unit (English) .............................. 4Définition des symboles apparaissant sur l’appareil (Français) ........... 4

Symbol Definitions .................................................................... 4Símbolos que Aparecen en la Unidad (Español) ................................. 4Definitionen der am Gerät angebrachten Symbole (Deutsch) .............. 4

Safety Precautions .................................................................... 5Chemical Handling .............................................................................. 5

Ammonium Chloride .................................................................................................. 5Aluminum Chloride ..................................................................................................... 5

Feature and Control Locations .................................................. 6Specifications ............................................................................ 8Typical Applications for the Vapor Sublimation Trap .................. 9About the HPSTM Vapor Sublimation Trap ................................ 10Installing the Vapor Sublimation Trap ...................................... 11

Orienting the Trap ...............................................................................11Locating the Trap ................................................................................11Wet Pump ..........................................................................................11Dry Pump ...........................................................................................12Using Cooling Water ...........................................................................13

Maintaining the Vapor Sublimation Trap .................................. 14Cleaning the Trap ................................................................................14NH4Cl.................................................................................................14AlCl3 ..................................................................................................14Drying the Trap ...................................................................................15Waste Management ...........................................................................15

Accessories / Part Replacement ............................................. 16Product Warranty ..................................................................... 17Notes ....................................................................................... 18


Appendix A: ......................... A.1 Vapor Pressure Curves ...... A.1

NH4Cl A.1AlCl3 A.2

1Vapor Sublimation TrapVapor Sublimation TrapVapor Sublimation TrapVapor Sublimation TrapVapor Sublimation Trap

The first two symbols, that may be located on your HPSTM, VaporSimulation Trap identify critical safety concerns. They are usedthroughout this manual to further define the safety concerns associatedwith the product.

The last two symbols identify other information in this manual that isessential or useful in achieving optimal performance from the HPSTM,Vapor Simulation Trap.

Package Contents

Symbols Used in this Manual

Before unpacking your Vapor Sublimation Trap, check all surfaces of thepacking material for shipping damage.

Please be sure that your Vapor Trap package contains these items:

1 Trap unit

1 HPS™ Vapor Sublimation Trap User's Manual

Inspect the Trap for visible evidence of damage. If it has been damaged inshipping, notify the carrier immediately. Keep all shipping materials andpackaging 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.

t

t

2 Vapor Sublimation TrapVapor Sublimation TrapVapor Sublimation TrapVapor Sublimation TrapVapor Sublimation Trap2

Definitions of CAUTION andNOTE messages used throughoutthe manual.

CAUTION: Refer toaccompanying documents.ISO 3864, No. B.3.1

This sign denotes a hazard.It calls attention to aprocedure, practice,condition, or the like, which,if not correctly performed oradhered to, could result ininjury to personnel.

This sign denotes a hazard.It calls attention to anoperating procedure,practice, or the like, which, ifnot correctly performed oradhered to, could result indamage to or destruction ofall or part of the product.

This sign denotes importantinformation. It calls attentionto a procedure, practice,condition, or the like, whichis essential to highlight.

Safety Information

Définition des indicationsATTENTION et REMARQUEutilisées dans ce manuel.

ATTENTION: Se reporter à ladocumentation. ISO 3864, No. B.3.1

L’indication signale un dangerpotentiel. Elle est destinée à attirerl’attention sur une procédure, uneutilisation, une situation ou touteautre chose présentant un risque deblessure en cas d’exécutionincorrecte ou de non-respect desconsignes.

L’indication signale un dangerpotentiel. Elle est destinée à attirerl’attention sur une procédure, uneutilisation, une situation ou touteautre chose présentant un risqued’endommagement ou de dégâtd’une partie ou de la totalité del’appareil en cas d’exécutionincorrecte ou de non-respect desconsignes.

L’indication REMARQUE signaledes informations importantes. Elleest destinée à attirer l’attention surune procédure, une utilisation, unesituation ou toute autre choseprésentant un intérêt particulier.

Symbols Used in thisManual(English)

Symboles utilisés dansce manuel(Français)


Definiton der mit VORICHT! undHINWEIS überschriebenenAbschnitte in dieserBetriebsanleitung.

VORSICHT! Bitte Begleitdokumentelesen! ISO 3864, Nr. B.3.1

Das Symbol VORSICHT! weist aufeine Gefahrenquelle hin. Es machtauf einen Arbeitsablauf, eineArbeitsweise, einen Zustand odereine sonstige Gegebenheitaufmerksam, deren unsachgemäßeAusführung bzw. UngenügendeBerücksichtigung zuKörperverletzung führen kann.

Das Symbol VORSICHT! weist aufeine Gefahrenquelle hin. Es machtauf einen Bedienungsablauf, eineArbeitsweise oder eine sonstigeGegebenheit aufmerksam, derenunsachgemäße Ausführung bzw.Ungenügende Berücksichtigung zueiner Beschädigung oderZerstörung des Produkts oder vonTeilen des Produkts führen kann.

Das Symbol HINWEIS weist aufeine wichtige Mitteilung hin, dieauf einen Arbeitsablauf, eineArbeitsweise, einen Zustand odereine sonstige Gegebenheit vonbesonderer Wichtigkeitaufmerksam macht.

Definiciones de los mensajes dePRECAUCIÓN y OBSERVACIÓNusados en el manual.

PRECAUCIÓN: Consultar los docu-mentos adjuntos. ISO 3864, N.° B.3.1

Esto símbolo indica un riesgo. Ponede relieve un procedimiento,práctica, condición, etc., que, de norealizarse u observarsecorrectamente, podría causarlesiones a los empleados.

Esto símbolo indica un riesgo.Pone de relieve un procedimiento,práctica, etc., de tipo operativoque, de no realizarse u observarsecorrectamente, podría causardesperfectos al instrumento, ollegar incluso a causar sudestrucción total o parcial.

Esto símbolo indica informaciónde importancia. Pone de relieveun procedimiento, práctica,condición, etc., cuyoconocimiento resulta esencial.

In dieserBetriebsanleitungvorkommendeSymbole (Deutsch)

Símbolos Usados en elManual (Español)


Attentionse reporter à la documentationISO 3864, No. B.3.1

Attentionsurface brûlanteIEC 417, No. 5041

Masse, ChâssisIEC 417, No. 5020

Matériel de la Classe IIIEC 417, No. 5172-a

Cautionrefer to accompanying documentsISO 3864, No. B.3.1

Cautionhot surfaceIEC 417, No. 5041

Frame or ChassisIEC 417, No. 5020

Class II EquipmentIEC 417, No. 5172-a

PrecauciónConsultar los documentosadjuntosISO 3864, N.° B.3.1

PrecauciónSuperficie calienteIEC 417, N.° 5041

Caja o chasisIEC 417, N.° 5020

Equipo de clase IIIEC 417, N.° 5172-a

Vorsicht!Bitte Begleitdokumentelesen!ISO 3864, Nr. B.3.1

Vorsicht!Heiße Fläche!IEC 417, Nr. 5041

Rahmen oder ChassisIEC 417, Nr. 5020

Geräteklasse IIIEC 417, Nr. 5172-a

Symbol Definitions

Definition ofSymbols Foundon the Unit(English)

Définition des symbolesapparaissant surl’appareil (Français)

Definitionen der amGerät angebrachtenSymbole (Deutsch)

Símbolos que Aparecenen la Unidad (Español)


Safety Precautions

The following general safety precautions must be observed during allphases of operation of this product. Failure to comply with theseprecautions or with specific warnings elsewhere in this manual violatessafety standards of intended use and may impair the protection provided bythe equipment. HPS Division of MKS Instruments, Inc. assumes no liabilityfor 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 skinabsorption. 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 resistantgloves, safety goggles, and other protective clothing. Wash up thoroughlyafter handling the chemical.

NH4Cl is corrosive and soluble in water.

Aluminum Chloride

AlCl 3 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 resistantgloves, safety goggles, and other protective clothing. Wash up thoroughlyafter handling the chemical.

AlCl3 is corrosive and reacts violently with water.


x

y

x

y

x

y

x

y

NW 50 Angle Trap

NW 50 Offset, Inline Trap

NW 80 Angle Trap

NW 80 Off-Set, Inline Trap

Feature and Control Locations


6" BODY 8"BODY

INLINE X Y X Y

NW 50 9.5 10.5 9.2 12.3(241) (267) (234) (312)

NW 80 8.0 9.3 7.8 11.0(203) (236) (198) (279)

NW 100 7.3 9.3 7.0 11.0(185) (236) (178) (279)

ANGLE X Y X Y

NW 50 7.0 7.8 6.7 9.5(178) (198) (170) (241)

NW 80 5.3 6.0 5.0 7.8(135) (152) (127) (198)

NW 100 5.0 5.0 4.3 6.8(127) (127) (109) (173)

x

yx

y

NW 100 Angle Trap

NW 100 Off-Set, Inline Trap

DIMENSIONS IN.(MM)


Specifications

Body Diameter

Capacity

6-inch

8-inch

Efficiency

Flow Conductance(Viscous Flow Region)

Pressure Drop Across Trap(Viscous Flow Region)

Cooling Water Flow Rate

Cooling Water Temperature

Materials

Flanges/Interface

Typical Dry Weight with MFFlanges

6-inch

8-inch

Design and/or specifications subject to change without notice.

6 or 8 in.

3.0 lb (1.4 kg) NH4Cl

4.5 lb (2.0 kg) AlCl3

10.0 lb (4.5 kg) NH4Cl

15.0 lb (6.8 kg) AlCl3

> 99 %

C (L/sec) = 20.74pp – pressure in mTorr

p (mTorr) = 812 Q/p2

Q – gas flow rate in sccmp – pressure in mTorr

> 6 gal/hr (400 mL/min)

< 86°F (30°C), lower is better

304 and 316 series stainless steel,elastomer seal

MF 100, MF 80KF 100, KF 80, KF 50Reducers are required and availablefor MF 63 and KF 40 pump lines

16.5 lb (7.5 kg)

28.0 lb (12.7 kg)


Typical Applications for theVapor Sublimation Trap

vv

vv

vv

Collect ammonium chloride (NH4Cl) in a silicon nitride CVD system

Collect aluminum chloride (AlCl3) in an aluminum etching system

Trap condensable vapors that begin to solidify aboveambient temperature


About the HPSTM

Vapor Sublimation TrapCHEMICAL REACTION PROCESSES, such as Chemical Vapor Deposition (CVD),are carried out under high temperature and vacuum conditions such that ahigh reaction rate can be reached and particulate contamination lessened.Ammonium chloride (NH

4Cl) by-product from silicon nitride

CVD and aluminum chloride (AlCl3) by-product

from aluminum etching solidifyabove ambient temperature.Resulting clogged pump linesand contaminated systemsrequire frequent maintenance.

The HPS™ VaporSublimation Trap collectsthese condensable vapors,significantly reducingmaintenance and increasingthroughput. Its efficiencyrating of more than 99% andhigh capacity ensure lessdown time and higherproduct yield, making itespecially desirable to thesemiconductor industry.

The Trap is designed withtwo stages — the first for highcapacity, the second forattaining high trappingefficiency. The first stage, atthe entrance of the Trap, has ahigher volume for collectingcondensable by-product thancomparable traps. In fact, itscapacity is approximately 5 to 10times greater than other traps ofthe same class.

Several perforated stainless steel conesare placed in the second stage to maximizethe heat transfer between the gas and coolingsurface while maintaining the necessary high flowconductance. This is a final “polish” of the gas flow.


Installing theVapor Sublimation Trap

Orienting the Trap

The orientation of the Trap has a negligible effect on the performance of theTrap as the condensed ammonium chloride and aluminum chloride are veryhard, dense materials.

The Vapor Trap must be installed in the correct flow direction,indicated by the arrow sign on the Trap body, to attain itshighest capacity and efficiency.

Locating the Trap

Figure 1 at the bottom and figure 2 on the next page show Trap installationsuggestions for a wet pump and a dry pump, respectively. Shaded areasrepresent heated lines or components, while unshaded areas representunheated or cold lines or components.

Wet Pump

As shown in figure 1A, when the Trap is installed next to a wet pump andnot in a clean room, replacement of the Trap is greatly simplified.

Figure 1B shows the Trap located just downstream of a heated isolationvalve. 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


Dry Pump

Though a trap is not required with a dry pump (figure 2A), one should beused 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 Scrubberload is reduced dramatically and heated lines post-Trap are not needed sincemost of the condensable vapors have been collected in the Trap.

In figures 2C and 2D, the Trap is installed upstream of the pump to preventsolidified vapors from clogging or damaging it. This option also reduces theamount of ballast nitrogen dramatically, thus improving both theperformance and lifetime of the dry pump.

With a Trap, you can use an unheated roots blower to achieve higherpumping speed and lower the ultimate pressure in a CVD system.

General rules for locating the Trap are:

Apply heat to the pump line between the reaction chamber andthe Trap,

Place a heated isolation valve between the reaction chamber andthe Trap, and

Install the Trap more than 3 feet away from the exit of thereaction chamber.

v

v

v

Figure 2: Installation options with a dry pump.

A

B

C

D


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 shouldbe kept at approximately 6 gallons per hour or higher. The temperature ofthe cooling water should be less than 30°C, a lower water temperature ispreferred.

Vapor pressure curves for both ammonium chloride and aluminum chlorideare shown in Appendix A. These curves show at what temperatures heatedlines located before the Trap operate most efficiently as a function ofpressure, as well as the partial pressure of the condensable vapor leavingthe Trap.


Maintaining theVapor Sublimation TrapSince the Vapor Trap is used to collect such by-products as solidifiedammonium chloride (NH

4Cl) or aluminum chloride (AlCl

3), the conductance

of the Trap will decrease after a period of operation. Eventually, the Trapwill limit gas flow rate due to the condensed solid, and periodical cleaning ina water bath with follow-up baking is necessary.

Cleaning the Trap

NH4Cl

Since NH4Cl is soluble in water, clean the Trap in a water bath.

Mechanical cleaning is not recommended since solidified NH4Cl is a

very strong, harsh material.

Do not attempt to separate internal from trap body prior tocleaning. Failing to do so may result in significant damageto the trap.

1 Insert the Trap into a fresh, circulating warm water bath. Since thesolubility of NH

4Cl 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 tolower the acidity of the solution for minimal corrosion. A fresh waterpressurized rinse is preferred.

Do not use hot water. HCl acid may be generated during thedissolving process prematurely corroding the Trap body.

3 When removing internasal from body, be sure to pull internalout axially do not spin or twist the internal, or damage to thecoils could result.

AlCl 3

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 NH

4Cl. High levels of

HCl acid will be generated if hot water is used.

AlCl 3 reacts violently with water. Special safety proceduresshould be followed during the cleaning process.


Drying the Trap

Place the Trap in an oven to dry for about 2 hours after cleaning in thewater bath. Set the oven temperature to less than 120°C. A highertemperature may vaporize the water concealed in the cooling coils by thequick-release couplings.

Since large amounts of by-product are collected in the Trap, it may takeseveral hours to complete the whole cleaning and drying process.

It is highly recommended that a spare Trap be available andused to replace the other during cleaning to minimizedowntime. Water vapor contamination, due to environmentexposure, will also be reduced.

Waste Management

Please consult with your local waste management authorities for properdisposal of hazardous chemical waste.


1

Accessories / Part Replacement

Part #Replacement Internal

6-inch Body 1000049548-inch Body 100009608

Bonnet Flange Sea l

For 6-inch BodyViton® 100003597Silicone 100004790

For 8-inch BodyViton® 100762020Silicone 100009637

Self-Sealing, Quick-Release H 2O Fitting

Straight, Qty 2 10000498090° Elbow, Qty 2 100004981

Please call HPSTM' Customer Service Department at 1-303-449-9861 or1-800-345-1967 to order any of these accessories or to receive catalogs forother HPSTM Products.


Product Warranty

Extent of the WarrantyMKS Instruments, Inc., warrants the HPSTM 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 authorizedrepresentative to the original purchaser (PURCHASER). Any product or parts of the product repaired orreplaced 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 becharged HPSTM’ current prices for parts and labor, plus any transportation for any repairs or replacement.

ALL EXPRESS AND IMPLIED WARRANTIES, INCLUDING THE IMPLIED WARRANTIES OFMERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE, ARE LIMITED TO THE WARRANTYPERIOD. NO WARRANTIES, EXPRESS OR IMPLIED, WILL APPLY AFTER THIS PERIOD.

Warranty ServiceThe 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 purchaseprice.

What Is Not CoveredThe 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 periodof 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 orthird parties not authorized in the manual.

Condition of Returned ProductsHPSTM 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 contaminatedwith 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 ofhumans, or is environmentally unsafe, it is the responsibility of the PURCHASER to have the productcleaned by an independent agency skilled and approved in the handling and cleaning of contaminatedmaterials 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 thePURCHASER 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 returnauthorization. Notwithstanding such inquiries, it is the responsibility of the PURCHASER to ensure that noproducts are returned to HPSTM which have been contaminated in the aforementioned manner.

Other Rights and RemediesI. These remedies are exclusive. HPSTM SHALL NOT BE LIABLE FOR CONSEQUENTIAL DAMAGES,

FOR ANTICIPATED OR LOST PROFITS, INCIDENTAL DAMAGES OR LOSS OF TIME, OR OTHERLOSSES INCURRED BY THE PURCHASER OR BY ANY THIRD PARTY IN CONNECTION WITHTHE PRODUCT COVERED BY THIS WARRANTY, OR OTHERWISE. Some states do not allowexclusion or limitation of incidental or consequential damage or do not allow the limitation on howlong an implied warranty lasts. If such laws apply, the limitations or exclusions expressed hereinmay not apply to PURCHASER.

II. Unless otherwise explicitly agreed in writing, it is understood that these are the only writtenwarranties given by HPSTM. Any statements made by any persons, including representatives ofHPSTM, which are inconsistent or in conflict with the terms of the warranty shall not be binding onHPSTM 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 rightswhich vary from state to state.

IV. For HPSTM products sold outside of the U.S., contact your MKS representative for warrantyinformation and service.

Warranty PerformanceTo 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 presentproof of original purchase.


Notes

Vapor Sublimation Trap A.1

Appendix A: Vapor Pressure Curves

NH4Cl

0 50 100 150 200 250 300 350

Temperature(°C)

Pre

ssur

e(T

orr)

103

102

101

100

10-1

10-2

10-3

10-4

10-5

Solid Phase

Vapor Phase

Vapor Sublimation TrapA.2

103

102

101

100

10-1

10-2

10-3

10-4

10-5

Temperature(°C)

0 50 100 150 200

Pre

ssur

e(T

orr)

Vapor Phase

Solid Phase

AlCl3

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