EP0924487B1 - Séchage à vide de matériau semi-conducteur - Google Patents

Séchage à vide de matériau semi-conducteur Download PDF

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Publication number
EP0924487B1
EP0924487B1 EP98124206A EP98124206A EP0924487B1 EP 0924487 B1 EP0924487 B1 EP 0924487B1 EP 98124206 A EP98124206 A EP 98124206A EP 98124206 A EP98124206 A EP 98124206A EP 0924487 B1 EP0924487 B1 EP 0924487B1
Authority
EP
European Patent Office
Prior art keywords
semiconductor
drying
semiconductor material
vacuum
vacuum drying
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP98124206A
Other languages
German (de)
English (en)
Other versions
EP0924487A3 (fr
EP0924487A2 (fr
Inventor
Wilhelm Schmidbauer
Hanns Dr. Wochner
Werner Ott
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wacker Chemie AG
Original Assignee
Wacker Chemie AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wacker Chemie AG filed Critical Wacker Chemie AG
Publication of EP0924487A2 publication Critical patent/EP0924487A2/fr
Publication of EP0924487A3 publication Critical patent/EP0924487A3/fr
Application granted granted Critical
Publication of EP0924487B1 publication Critical patent/EP0924487B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum

Definitions

  • the invention relates to a method for drying Semiconductor broken material.
  • semiconductor material is, for example, semiconductor material, such as silicon, indium phosphide, germanium, gallium arsenide or gallium phosphide.
  • the targeted dopants are the only "contaminants" which is the cheapest such material Case should have. One tries therefore the concentrations harmful contaminants as low as possible hold.
  • the JP-A-63-302251 discloses a method for cleaning and drying of silicon wafers, taking a vacuum during drying is created.
  • High-purity silicon is obtained by chemical conversion of the Raw silicon into a liquid silicon compound (for example Trichlorosilane) using distillation processes can be processed in the purest form. In a subsequent one chemical deposition process, this becomes highly pure Silicon compound then converted into high-purity silicon. It falls as polycrystalline silicon in the form of rods as an intermediate.
  • a liquid silicon compound for example Trichlorosilane
  • the majority of the polycrystalline semiconductor material is used for the production of crucible-grown single crystals, from Tapes and foils or for the production of polycrystalline Solar cell base material used.
  • the polycrystalline semiconductor material such as mentioned polycrystalline silicon rods
  • single-crystalline ones Semiconductor recycling material before melting crushed. This is usually always with a superficial Contamination of the broken semiconductor material, because the crushing mainly with mechanical crushing tools, such as metallic or ceramic jaw or roller crushers, Hammering or chiseling. Through the crushing process foreign atoms (iron, chromium, nickel, copper etc.) worked into the surface of the semiconductor material or stick to the surface. But also with the alternatives Crushing processes, e.g. Water jet breaking, shock wave crushing etc., it cannot be entirely excluded that such contaminations with foreign atoms occur or that harmful dust and / or particles on the fracture surface can reach.
  • contamination by metal atoms is critical to look at, as these the electrical properties of the Can change semiconductor material in a harmful way. Dust and / or particles on the surface can sustain the affect the subsequent drawing process (dislocations, etc.).
  • the semiconductor fragments have to be melted before melting chemical surface treatment with subsequent cleaning and subjected to drying to the specified purity values to reach the surface.
  • the surface of the machined semiconductor material with various acids such as a mixture etched from nitric acid and hydrofluoric acid. This Procedure is widely used. After that, usually the semiconductor breakage material, such as polycrystalline Silicon breakage, rinsed with ultrapure water and dried. There no contamination in the crucible with the semiconductor material the surface / surface structure of the semiconductor broken material absolutely dry, dust, stain and be acid free.
  • the semiconductor breakage material such as polycrystalline Silicon breakage
  • Semiconductor material is usually very brittle, which is why it is formed through the breaking process a sharp, jagged Semiconductor breakage material with a large number of fine hairline cracks, which spreads to the cm area below the surface to have. In particular, these cracks form due to the Capillary action Residual moisture (water, acid residues) in the Afterwards for contamination (stains) i.e. to committee material or even lead to burns.
  • contamination i.e. to committee material or even lead to burns.
  • To meet the high quality requirements, which are constantly being tightened to meet is a perfect drying, i.e. acid and stain free Semiconductor broken material, absolutely necessary.
  • the conventional convection drying (the material to be dried is overflowed or with pure air) does not bring hoped for success in a timely manner (under a Hour), which includes recognizable by the color of litmus paper is, unless that is complex, voluminous and therefore expensive Facilities are built, or the goods are stored unpacked for a longer period "outdoors", the Risk of increased dust contamination is very high.
  • Another disadvantage of convection drying is that Moisture remains in the finest hairline cracks and so does that Risk of subsequent staining / dust pollution increased becomes.
  • the upper layer is primarily used for radiation drying heated so that areas on the "shadow side" of the semiconductor fragments or deeper layers in the case of fillings cannot be recorded sufficiently. Furthermore is one Acid removal from the hairline cracks not given properly. This also leads to staining, that is to say Committee material.
  • the radiation intensity is increased, i.e. the surface temperature is increased to over 100 ° C, then diffuse at increasing temperature not cleaned metal ions in the Surface of the broken semiconductor material and contaminate sustainably the pure semiconductor material. This leads to a Decline in quality, if necessary, to committee.
  • Drum drying is not practical either because of the Movement of the piece goods between broken semiconductor material and process drum or on the other hand between the semiconductor fragments Sustainable drum abrasion or semiconductor fine breakage / dust itself arises, whereby the following Drawing process is severely impaired (high dislocation rate) and also leads to rejects.
  • the object of the invention is to overcome the disadvantages of the prior art Technology to overcome, especially a dust, stain and to enable acid-free drying of semiconductor fragments, doing this in an efficient and economical Way is done.
  • the object is a method for drying semiconductor broken material by means of vacuum, which is characterized that drying by applying a vacuum several times in Change with flooding with ultrapure air and / or inertizing Gases.
  • the semiconductor broken material preheated from the final cleaning with ultrapure water which is preferably 80 ° C., is dried in a vacuum drying chamber, preferably described above.
  • This vacuum drying chamber is preferably with the help of a vacuum pump with high suction power to a pressure of 10 -2 mbar to 10 -5 .
  • the suction power ranging from 30 m 3 / h to 250 m 3 / h, preferably 100 to 200 m 3 / h (the suction power depends, inter alia, on the number of to be dried Receiving devices (process trays) and the amount of broken semiconductor material to be dried (the product throughput), the material layering (single-layer or multi-layered) or the semiconductor broken structure / size, ie the resulting vacuum drying chamber size.
  • this evacuation process preferably allows the residual moisture to be removed from the so-called hairline cracks in the broken semiconductor materials.
  • the vacuum drying chamber After the vacuum drying chamber is evacuated, it is cleaned with dry, pure air with a relative humidity of less than 20% or pure, inertizing gases (e.g. nitrogen, argon etc.) at a temperature of 20 to 90 ° C, preferably approx. 80 ° C and a gas Volume flow of preferably 2 to 20 m 3 / h flooded.
  • inertizing gases e.g. nitrogen, argon etc.
  • the interplay of evacuation and flooding with ultrapure air and / or pure inert gas is preferably carried out 1 to 3 times, inter alia depending on the size and / or structure of the fracture.
  • the broken semiconductor material is forced to flow through during flooding or evacuation; this promotes the moisture absorption of the ultrapure air and / or the inert gas and accelerates and intensifies the drying process.
  • the evacuation and flooding of the vacuum drying chamber preferably takes 5 to 60 minutes. at a throughput of 250 kg / h (depending on the size of the vacuum chamber, the size of the fracture and / or the structure of the fracture, among other things).
  • the pure air / gas volume flow is preferably in a range from 2 to 20 m 3 / h.
  • vacuum drying can depends on the Fracture size and / or structure (as predrying) another one preceded by conventional convection drying, in which the Recording device also preferably with dry pure air with a relative humidity of less than 20% and a temperature of 20 to 90 ° C preferred is flowed through from 60 to 90 ° C.
  • the influx of pure air is preferably carried out over a laminar airflow ceiling.
  • vacuum drying is done alone, it is preferably 10 min to 60 min. If convection drying is required, the total drying time is preferably 20 minutes up to 120 min. These times refer to throughput of semiconductor fragments of preferably 250 kg / h.
  • the semiconductor breakage material about a subsequent foreclosed Transport route which is preferably a conventional laminar flow ceiling of the clean room class 10 to 1000, on one cooled to a maximum temperature of 30 ° C before being in a Packaging device is welded in foil.
  • the process line is preferably with a laminar airflow ceiling, for example the RR class 100, built over.
  • the advantage of vacuum drying is that of drying by means of the usual convection / radiation drying in it, that complete drying of the semiconductor debris at temperatures below 100 ° C is possible.
  • no temperatures above 100 ° C are required are the disadvantageous diffusion process of foreign metal ions in the semiconductor material - as with the Radiation drying - next to nothing. It can therefore be a Semiconductor broken material are produced, which the highest quality requirements enough.
  • the drying device clearly can be reduced, thereby saving production space becomes.
  • conventional convection drying involves several Meters, whereas vacuum drying in the meter range lies.
  • the size and scope of the climate technology can also be determined here and clean room technical facilities accordingly significantly reduce, in particular investment costs but also ongoing operating / energy costs saved can be.
  • Vacuum drying can be done due to its small spatial Advantageously build dimensions in modular construction and thus relatively easy in the existing production processes install.
  • a Appropriate device that with at least one vacuum-tight device at least one receiving device for broken semiconductor material and that there is a vacuum in the device can.
  • the device for drying broken semiconductor material has at least one vacuum-tight device, which can be a vacuum drying chamber, which has a lid which can be opened to introduce the broken semiconductor material and which can be closed in a vacuum-tight manner, the vacuum drying chamber preferably being wall-heated.
  • a vacuum pump with high suction power which generates a pressure of 10 -2 to 10 -5 mbar, preferably 10 -3 to 10 -4 mbar, and a suction power of 30 m 3 / h to 250 m 3 / h , preferably 100 m 3 / h to 200 m 3 / h (the suction power is dependent, among other things, on the number of receiving devices to be dried (process trays) and the amount of broken semiconductor material to be dried (the product throughput), the material layering (single-layer or multi-layer) or the semiconductor fracture structure / size, ie the resulting vacuum drying chamber size).
  • a receiving device is preferably used, which preferably has openings, these openings preferably being in the bottom (perforated bottom), in which the semiconductor broken material is located, which preferably has a grain size distribution of 2 mm to 150 mm.
  • This vacuum drying chamber is preferably a container made of VA-2 or VA-4 steel, which is either electropolished or lined with clean room-compatible and temperature-resistant materials such as preferably silicon or the plastics Teflon and PFA.
  • the receiving device used (process shell) is seated on a sealing strip, so that the receiving device, ie the broken semiconductor material, is forced to flow through the perforated bottom with heated pure air and / or pure inert gas.
  • the cycle time is preferably in a range from 2 to 10 minutes. (inter alia depending on the fracture structure, size, suction power of the vacuum pump, quantity used and the gas volume flow).
  • This vacuum drying chamber can (as it were for pre-drying) also a conventional device for convection drying precede, this device being a chamber through from above through preferably a temperature-resistant laminar airflow ceiling dry ultrapure air with a humidity less than 20% and with a temperature of 60 to 100 ° C, can preferably flow from 70 to 90 ° C.
  • Their use and the drying time depends on the amount and type of Material (fraction size / structure) and is at a throughput from 250 kg / h, preferably 0 min to 1 h.

Landscapes

  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Drying Of Solid Materials (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Claims (3)

  1. Procédé de séchage de matériau de fragments semi-conducteurs à l'aide d'un vide, caractérisé en ce que le séchage se fait par une application à plusieurs reprises d'un vide, en alternance avec la purge à l'aide d'air ultra pur et/ou de gaz à capacité d'inertisation.
  2. Procédé de séchage de matériau de fragments semi-conducteurs à l'aide d'un vide selon la revendication 1, caractérisé en ce que le matériau de fragments semi-conducteurs est séché auparavant tout au moins à l'aide d'un séchage par convection.
  3. Procédé de séchage de matériau de fragments semi-conducteurs selon la revendication 1 ou 2, caractérisé en ce que l'air ultra pur sec et/ou les gaz à capacité d'inertisation présentent une humidité relative inférieure à 20%.
EP98124206A 1997-12-19 1998-12-17 Séchage à vide de matériau semi-conducteur Expired - Lifetime EP0924487B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19756830 1997-12-19
DE19756830A DE19756830A1 (de) 1997-12-19 1997-12-19 Vakuumtechnisches Trocknen von Halbleiterbruch

Publications (3)

Publication Number Publication Date
EP0924487A2 EP0924487A2 (fr) 1999-06-23
EP0924487A3 EP0924487A3 (fr) 1999-07-07
EP0924487B1 true EP0924487B1 (fr) 2001-02-14

Family

ID=7852715

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98124206A Expired - Lifetime EP0924487B1 (fr) 1997-12-19 1998-12-17 Séchage à vide de matériau semi-conducteur

Country Status (4)

Country Link
US (1) US6170171B1 (fr)
EP (1) EP0924487B1 (fr)
JP (1) JPH11265875A (fr)
DE (2) DE19756830A1 (fr)

Families Citing this family (13)

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Publication number Priority date Publication date Assignee Title
US7270706B2 (en) * 2004-10-04 2007-09-18 Dow Corning Corporation Roll crusher to produce high purity polycrystalline silicon chips
FR2920046A1 (fr) * 2007-08-13 2009-02-20 Alcatel Lucent Sas Procede de post-traitement d'un support de transport pour le convoyage et le stockage atmospherique de substrats semi-conducteurs, et station de post-traitement pour la mise en oeuvre d'un tel procede
CN101561218B (zh) * 2008-04-16 2010-12-08 富葵精密组件(深圳)有限公司 真空氮气烘箱
US8756826B2 (en) * 2010-11-30 2014-06-24 Mei, Llc Liquid coalescence and vacuum dryer system and method
DE102011004916B4 (de) 2011-03-01 2013-11-28 Wacker Chemie Ag Vorrichtung und Verfahren zum Trocknen von Polysilicium
US11713924B2 (en) 2012-02-01 2023-08-01 Revive Electronics, LLC Methods and apparatuses for drying electronic devices
US10876792B2 (en) 2012-02-01 2020-12-29 Revive Electronics, LLC Methods and apparatuses for drying electronic devices
US9970708B2 (en) 2012-02-01 2018-05-15 Revive Electronics, LLC Methods and apparatuses for drying electronic devices
US10240867B2 (en) 2012-02-01 2019-03-26 Revive Electronics, LLC Methods and apparatuses for drying electronic devices
US10690413B2 (en) 2012-02-01 2020-06-23 Revive Electronics, LLC Methods and apparatuses for drying electronic devices
DE102012218748B4 (de) 2012-10-15 2014-02-13 Wacker Chemie Ag Trocknen von Polysilicium
US10088230B2 (en) 2012-11-08 2018-10-02 Tekdry International, Inc. Dryer for portable electronics
WO2014153007A1 (fr) 2013-03-14 2014-09-25 Revive Electronics, LLC Procédés et appareils pour des dispositifs électroniques de séchage

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US4816081A (en) * 1987-02-17 1989-03-28 Fsi Corporation Apparatus and process for static drying of substrates
JPS63302521A (ja) 1987-06-02 1988-12-09 Mitsubishi Electric Corp 半導体基板の乾燥装置
DE68910825T2 (de) 1989-09-15 1994-05-19 Ibm Verfahren und Vorrichtung zur Trocknung von Gegenständen.
FR2652888A1 (fr) 1989-10-06 1991-04-12 Annamasse Sa Ultrasons Procede de sechage sous vide de pieces diverses et dispositif de mise en óoeuvre du procede.
US5263264A (en) 1990-01-25 1993-11-23 Speedfam Clean System Company Limited Method and apparatus for drying wet work
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Also Published As

Publication number Publication date
EP0924487A3 (fr) 1999-07-07
EP0924487A2 (fr) 1999-06-23
DE59800476D1 (de) 2001-03-22
DE19756830A1 (de) 1999-07-01
JPH11265875A (ja) 1999-09-28
US6170171B1 (en) 2001-01-09

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