EP0757362A1 - Matériau de revêtement transparent aux rayons-X, procédé de fabrication et son emploi - Google Patents

Matériau de revêtement transparent aux rayons-X, procédé de fabrication et son emploi Download PDF

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Publication number
EP0757362A1
EP0757362A1 EP96112057A EP96112057A EP0757362A1 EP 0757362 A1 EP0757362 A1 EP 0757362A1 EP 96112057 A EP96112057 A EP 96112057A EP 96112057 A EP96112057 A EP 96112057A EP 0757362 A1 EP0757362 A1 EP 0757362A1
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EP
European Patent Office
Prior art keywords
protective layer
carrier material
beryllium
layer
coating
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.)
Withdrawn
Application number
EP96112057A
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German (de)
English (en)
Inventor
Martin Dr. Schmidt
Thomas Dr. Zetterer
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.)
Institut fuer Mikrotechnik Mainz GmbH
Original Assignee
Institut fuer Mikrotechnik Mainz GmbH
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 Institut fuer Mikrotechnik Mainz GmbH filed Critical Institut fuer Mikrotechnik Mainz GmbH
Publication of EP0757362A1 publication Critical patent/EP0757362A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/10—Scattering devices; Absorbing devices; Ionising radiation filters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J35/00—X-ray tubes
    • H01J35/02—Details
    • H01J35/16—Vessels; Containers; Shields associated therewith
    • H01J35/18—Windows

Definitions

  • the invention relates to an X-ray permeable layer material with a beryllium carrier material and the use of the layer material and a method for its production.
  • X-ray transmission windows made of beryllium and thin beryllium layers as base supports for the mask technique in X-ray lithography have long been known. Due to the low atomic number and thus a high transmission with regard to electromagnetic radiation in the X-ray range and a high mechanical strength, the metal beryllium is excellently suitable both as a window material and as a carrier material for structured absorber layers. The material is able, despite the use of relatively small layer thicknesses and thus high transmission of radiation in the X-ray range, high pressure differences, e.g. in vacuum-atmosphere transitions to withstand safely.
  • beryllium has the crucial disadvantage that it is not resistant to chemicals. This creates when used in conjunction with ionizing radiation and atmospheric oxygen or in the vicinity of aqueous solutions, e.g. during the creation of absorber structures for X-ray (deep) lithography, the extremely toxic beryllium oxide.
  • Beryllium substrates are known, which by evaporation or sputtering of metals, such as. Titan, are protected.
  • metals such as. Titan
  • Berner has the disadvantage of applying the metals by vapor deposition or sputtering that holes form at the points where the substrate has unevenness in the coating and therefore no isotropic coating can take place.
  • Another disadvantage is the lack of chemical resistance, e.g. against acids or acidic solutions.
  • US-A 5,226,067 has therefore developed a coating for optical devices made of beryllium and other low atomic number elements which are coated with amorphous borohydride (aB: H) or an amorphous borohydride alloy (aB: X: H), where X is another Element with a low atomic number.
  • aB: H amorphous borohydride
  • aB: X: H amorphous borohydride alloy
  • X another Element with a low atomic number.
  • These coatings show a high transmission of X-rays and are stable against non-oxidizing and oxidizing acids.
  • the coating is carried out using a CVD process, for example using B 2 H 6 as the process gas.
  • this process has the decisive disadvantage that boron acts as a dopant, for example for silicon or diamond, and the coating system is highly contaminated by the boron-containing gases.
  • the coating system is therefore no longer available to other processes and a separate system for the B: H: X coating must therefore be provided. For this reason and because of the costly purchase and disposal of the process gases, this process is very expensive.
  • Another disadvantage of this coating is that it has high hydrogen contents. This high hydrogen contents result in poorer mechanical properties and a lack of resistance to long-term behavior when irradiated with high-intensity X-rays, such as synchrotron radiation.
  • the materials used to coat the beryllium carrier material are silicon oxide, silicon nitride, silicon carbide, amorphous carbon or a combination of these substances.
  • the coating is applied by a CVD coating process. Depending on the process conditions, hydrogen is always incorporated into such processes. However, the hydrogen content of the protective layer should be as low as possible and has a proportion of not more than 20%, preferably not more than 10%.
  • the other process alternative is to apply the coating using a sputtering process. With this method, the hydrogen content of the protective layer is almost zero.
  • the protective layer preferably completely covers the surface of the carrier material.
  • the thickness of the protective layer is advantageously 300 to 500 nm.
  • Such layer material is used as an X-ray transmission window, mask membrane or blank mask.
  • Protective layers of this type result in high dimensional stability, are mechanically strong and relatively resistant to abrasion. Furthermore, the protective layer is compatible with further process steps. An example of this is the process of absorber structuring for X-ray (deep) lithography. In contrast to beryllium, the protective layer is not attacked by the chemical processes associated with absorber structuring due to its resistance.
  • the layer material also allows typical process steps from semiconductor technology, such as coating and etching back of adhesive and electroplating start layers, tempering processes, application and development of resist, etching processes, etc., and is reproducible in terms of its chemical and physical surface properties.
  • the beryllium windows and membranes are preferably coated by a plasma-assisted coating process.
  • Coating processes for the production of thin layers of silicon oxide, silicon nitride, silicon carbide and amorphous carbon and combinations of these materials include plasma-assisted CVD processes which, starting from gaseous compounds such as silane, ammonia, methane, etc., produce solid compounds at temperatures, where the starting compounds do not normally react with each other.
  • PECVD for example 375 kHz or 13.56 MHz
  • LPCVD process low-pressure CVD process
  • ECR microwave CVD
  • the substrates for the carrier material are, for example, round 4-inch disks, similar to the common Si wafers. They are preferably covered on both sides with a 300 to 500 nm thick layer. This thickness is limited on the one hand by the fact that it should completely cover the surface and, in addition, should have a certain mechanical strength. On the other hand, the upper limit of the thickness is that both the transmission is not significantly reduced and the production costs should not increase excessively.
  • the coating process takes 15-30 minutes to produce a 500 nm layer.
  • one side is coated first and then the other side of the carrier material, with the edges being partially coated.
  • the layers produced with plasma support at low temperatures are usually amorphous with different stoichiometric proportions of the starting elements.
  • a typical formulation of a silicon nitride layer describes with Si x N y : H z both the variable stoichiometric proportions of silicon and nitrogen, as well as the more or less strong incorporation of hydrogen depending on the process conditions or starting substances (A.Shermon: Chemical vapor deposition for microelectronics, Moyes Publ., 1987).
  • the hydrogen content in the coatings should not be more than 20%, since excessive hydrogen contents result in poor mechanical properties and uncertainties with regard to the long-term behavior under high-intensity radiation.
  • the hydrogen content is preferably not more than 10%. However, the lower the hydrogen content, the more advantageous it is.
  • the corresponding formulations for silicon oxide, silicon carbide and amorphous carbon are Si x O y : H z , Si x C y : H z and C x : H y .
  • the layers that can be produced with these processes have properties that come very close to those of the bulk material. Especially the chemical ones Properties are comparable, which is why protective layers made of chemically resistant and radiation-resistant materials such as silicon oxide, silicon nitride, silicon carbide and amorphous carbon can be used for passivation of beryllium surfaces.
  • Such layers can be produced using different methods.
  • the low-pressure CVD process and sputtering are also suitable processes. Both processes are almost isotropic coating processes.
  • the advantages of the low pressure CVD process are that very low hydrogen contents can be achieved and there is also the possibility to control the stress of the layers.
  • the second method the sputtering process
  • the coating with plasma support is particularly preferred because it combines several advantages, in particular with beryllium as the carrier material.
  • the coating especially one with plasma support, does not require temperatures that are higher than 350 ° C.
  • the beryllium disks which have previously been produced, for example, by a rolling process or have been cut out of rolled sheet metal and therefore are under possible residual stress, do not warp during the coating. Since it is an almost isotropic coating process, there are no holes or pores in the protective layer because of any unevenness in the Substrate surface to be completely coated.
  • the method also includes self-cleaning of the surfaces of water and volatile hydrocarbons prior to coating due to increased substrate temperatures.
  • the deposited layers show good adhesion shadows on the substrate surface. By applying a bias voltage to the substrate holder, contamination of the recipient by sputtering effects can be largely avoided.
  • the layer stress can be controlled by a suitable choice of the process parameters. This property is particularly important for thin membranes.
  • the so-called "thick" mask membranes can be produced as follows: First, substrates of the desired geometric shape are cut out of a rolled sheet metal that can be obtained commercially, for example by wire erosion. In order to keep the surface flat and smooth, the loading substrates are then lapped and / or polished. Before or after the lapping and / or polishing, an annealing process at about 750 ° C. and a period of, for example, 1 to 2 hours can also be introduced in order to relieve internal residual stresses which may be present in the loading substrates due to the rolling process.
  • FIGS. 1a and 1b show how the protective layer 4 is applied to the substrate 1 during the coating process.
  • the substrate 1 is first coated from one side 2, the edges 5 being at least partially coated at the same time, as shown in FIG. 1a. Subsequently, the substrate 1 is turned over and the rear side 3 of the substrate 1 is coated, the edges 5 again being partially coated. In this way, the substrate 1 is completely covered with the protective layer from all sides, as shown in FIG. 1b.
  • FIGS. 2a-2c show a comparison of a plasma-assisted coating process, for example the plasma-assisted CVD process, with a directional coating process, for example the thermal vapor deposition process.
  • Irregularities in the uncoated substrate 1, such as depressions (FIG. 1a) lead to a protective layer 4 in directional coating processes, which has defects and does not completely cover the substrate surface (FIG. 1b).
  • an undirected coating process such as the plasma-assisted CVD process, irregularities can also be sealed (Figure 1c).
  • the following example illustrates the present invention.
  • the PECVD (Plasma Enhanced Chemical Vapor Deposition) process was chosen as the coating process.
  • the gas supply was regulated so that 80 sccm SiH 4 , 80 sccm NH 3 and 2000 sccm N 2 continuously flow into the coating chamber.
  • the substrate temperature is controlled at 300 ° C.
  • the RF power is 30 watts at a frequency of 13.56 MHz.
  • a growth rate of 1 nm / s was typically achieved with these parameters.
  • the typical thickness of the layers produced in this way was 500 nm.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Chemical Vapour Deposition (AREA)
  • Preparing Plates And Mask In Photomechanical Process (AREA)
  • Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
EP96112057A 1995-08-02 1996-07-25 Matériau de revêtement transparent aux rayons-X, procédé de fabrication et son emploi Withdrawn EP0757362A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19528329 1995-08-02
DE19528329A DE19528329B4 (de) 1995-08-02 1995-08-02 Maskenblank und Verfahren zu seiner Herstellung

Publications (1)

Publication Number Publication Date
EP0757362A1 true EP0757362A1 (fr) 1997-02-05

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EP96112057A Withdrawn EP0757362A1 (fr) 1995-08-02 1996-07-25 Matériau de revêtement transparent aux rayons-X, procédé de fabrication et son emploi

Country Status (3)

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US (1) US5740228A (fr)
EP (1) EP0757362A1 (fr)
DE (1) DE19528329B4 (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10223113B4 (de) 2002-05-21 2007-09-13 Infineon Technologies Ag Verfahren zur Herstellung einer photolithographischen Maske
WO2004097882A1 (fr) * 2003-04-30 2004-11-11 Tuilaser Ag Membrane transparente pour des faisceaux de particules, a emissivite amelioree de rayonnement electromagnetique
US7570741B2 (en) 2003-08-06 2009-08-04 Contraband Detection Systems, L.L.C. Diamond based proton beam target for use in contraband detection systems
DE10356035B4 (de) * 2003-12-01 2008-01-03 Infineon Technologies Ag Verfahren zur Herstellung einer Photomaske
US7329620B1 (en) * 2004-10-08 2008-02-12 National Semiconductor Corporation System and method for providing an integrated circuit having increased radiation hardness and reliability
US8498381B2 (en) * 2010-10-07 2013-07-30 Moxtek, Inc. Polymer layer on X-ray window
US8929515B2 (en) 2011-02-23 2015-01-06 Moxtek, Inc. Multiple-size support for X-ray window
US9076628B2 (en) 2011-05-16 2015-07-07 Brigham Young University Variable radius taper x-ray window support structure
US8989354B2 (en) 2011-05-16 2015-03-24 Brigham Young University Carbon composite support structure
US9174412B2 (en) 2011-05-16 2015-11-03 Brigham Young University High strength carbon fiber composite wafers for microfabrication
US20180061608A1 (en) * 2017-09-28 2018-03-01 Oxford Instruments X-ray Technology Inc. Window member for an x-ray device

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3617788A (en) * 1968-09-14 1971-11-02 Philips Corp Method of vacuum-tight closure of thin beryllium windows and x-ray tube provided with such a window
JPS5782954A (en) * 1980-11-11 1982-05-24 Nec Corp X-ray window
US4685778A (en) * 1986-05-12 1987-08-11 Pollock David B Process for nuclear hardening optics and product produced thereby
JPH04107912A (ja) * 1990-08-29 1992-04-09 Fujitsu Ltd Ｘ線露光用マスク
US5226067A (en) 1992-03-06 1993-07-06 Brigham Young University Coating for preventing corrosion to beryllium x-ray windows and method of preparing

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4436797A (en) * 1982-06-30 1984-03-13 International Business Machines Corporation X-Ray mask
US5012500A (en) * 1987-12-29 1991-04-30 Canon Kabushiki Kaisha X-ray mask support member, X-ray mask, and X-ray exposure process using the X-ray mask
JPH0353200A (ja) * 1989-07-20 1991-03-07 Fujitsu Ltd Ｘ線露光装置の製造方法
JPH04299515A (ja) * 1991-03-27 1992-10-22 Shin Etsu Chem Co Ltd Ｘ線リソグラフィ−マスク用ｘ線透過膜およびその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3617788A (en) * 1968-09-14 1971-11-02 Philips Corp Method of vacuum-tight closure of thin beryllium windows and x-ray tube provided with such a window
JPS5782954A (en) * 1980-11-11 1982-05-24 Nec Corp X-ray window
US4685778A (en) * 1986-05-12 1987-08-11 Pollock David B Process for nuclear hardening optics and product produced thereby
JPH04107912A (ja) * 1990-08-29 1992-04-09 Fujitsu Ltd Ｘ線露光用マスク
US5226067A (en) 1992-03-06 1993-07-06 Brigham Young University Coating for preventing corrosion to beryllium x-ray windows and method of preparing

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 006, no. 164 (E - 127) 27 August 1982 (1982-08-27) *
PATENT ABSTRACTS OF JAPAN vol. 016, no. 347 (E - 1240) 27 July 1992 (1992-07-27) *

Also Published As

Publication number Publication date
DE19528329B4 (de) 2009-12-10
DE19528329A1 (de) 1997-02-06
US5740228A (en) 1998-04-14

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