EP0121707B1 - Verfahren zum Schleifen von gestaltlosem Aluminium-Oxyd - Google Patents

Verfahren zum Schleifen von gestaltlosem Aluminium-Oxyd Download PDF

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Publication number
EP0121707B1
EP0121707B1 EP19840101834 EP84101834A EP0121707B1 EP 0121707 B1 EP0121707 B1 EP 0121707B1 EP 19840101834 EP19840101834 EP 19840101834 EP 84101834 A EP84101834 A EP 84101834A EP 0121707 B1 EP0121707 B1 EP 0121707B1
Authority
EP
European Patent Office
Prior art keywords
aluminum oxide
polishing
oxide surface
citric acid
silicon dioxide
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
Application number
EP19840101834
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English (en)
French (fr)
Other versions
EP0121707A3 (en
EP0121707A2 (de
Inventor
Jagtar Singh Basi
Eric Mendel
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.)
International Business Machines Corp
Original Assignee
International Business Machines Corp
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 International Business Machines Corp filed Critical International Business Machines Corp
Publication of EP0121707A2 publication Critical patent/EP0121707A2/de
Publication of EP0121707A3 publication Critical patent/EP0121707A3/en
Application granted granted Critical
Publication of EP0121707B1 publication Critical patent/EP0121707B1/de
Expired legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces

Definitions

  • Aluminum oxide is a chemically non-reactive, relatively hard material. Polishing of-such films which have been deposited upon surfaces of mechanical parts have not been accomplished up to the present.
  • the method comprises the chemical-mechanical polishing of amorphous aluminum oxide surfaces to a high degree of perfection.
  • the aluminum oxide surfaces are continuously wetted with a water-citric acid slurry containing a soft abrasive material.
  • the continuously wiping of the aluminum oxide surface is accomplished with a firm surface using pressure while maintaining a relative movement between the aluminum oxide surface and the firm surface to remove the water-citric acid reacted aluminum oxide product from the high points of the aluminum oxide surface. This method is cointinued until a high degree of perfection of the surface is accomplished.
  • the slurry is typically composed of colloidal silicon dioxide dispersed in water containing citric acid.
  • Figure 1 illustrates a cross-sectional view of the mechanical part 25 to be polished by the polishing process of the present description.
  • the part 25 includes a substrate 8 and an amorphous aluminum oxide layer 9 of about 5 to 8 micrometres in thickness formed upon the substrate. It is preferred to utilize as the substrate 8 a combination of aluminum oxide and titanium carbide in a fine grain mixture that has been pressed and sintered or hot pressed. However, titanium carbide particles alone may be compressed into desired parts in a similar fashion.
  • the mixture is characterized by an average particle size of less than about 5 microns and preferably the particles are 1 to 2 microns in length.
  • the preferred mixture is in the range of about 60 to 80% aluminum oxide and 40 to 20% titanium carbide by weight.
  • the high density mixture has low porosity and exhibits improvement in Young's and Shear moduli of elasticity and modulus of rupture.
  • the materials are ground into powders of the desired particle sizes and mixed in the desired composition of about 80 to 60% aluminum oxide to 20 to 40% titanium carbide to a homogeneous mixture.
  • the dry powder is measured and poured to fill a graphite pressing mold.
  • the powder charge is then precompacted with an applied load of approximately 68.95 to 206.85 bar.
  • the precompacted mold is loaded into a hot press and heated to a temperature in the range of 1400°C to 1650°C.
  • the pressed part is hot pressed, when the desired temperature is reached at a pressure of between 275.8 and 413.7 bar.
  • the pressed part is cooled to room temperature for a desired time to maintain a stress-free condition.
  • the cooled part is removed from the mold, deburred and sand blasted to remove any excess graphite.
  • the part is now machined to the desired shape and dimensions using conventional diamond machining and mechanical lapping methods.
  • Amorphous aluminum oxide films can be deposited using chemical vapor deposition or rf sputtering methods.
  • the rf sputtering method entails the use of a dielectric target of high purity.
  • the target is metallized on one side and bonded to a flat water cooled aluminum disc using a silver epoxy bonding agent or other suitable conducting bonding agents.
  • the water cooled aluminum disc forms part of the vacuum chamber wall through a system of vacuum seals and an insulating ring.
  • a protective metal shield surrounds the exposed areas of the water cooled aluminum disc at an appropriate spacing of 0.5 cm in order to prevent sputtering from this region.
  • the source of power is an rf generator.
  • the polishing process for aluminum oxide or the like may be understood with reference to Figures 2 and 3.
  • the polishing machine includes a bowl 10 having a slurry outlet 12 and a driven plate 14. Mounted on the plate 14 by any suitable means (not shown) is a soft, firm surface or pad 16 composed of a poromeric material.
  • the pad materials used are true poromeric comprised of a top coat and substrate layer.
  • the thickness of the top coat is critical. Top coat thickness is 381-508 pm, substrate is 508-635 pm. Total package is 1022 ⁇ 50.8 pm thick.
  • the top coat is designed and made by a coagulation process to obtain a macro and micro pore random structure. The macro pores are irregularly shaped and randomly dispersed without any preferred orientation in the top coat layer.
  • the preferred pressure is between about 1.5x 1 04 to 4.25x10" Pa (about 150 to 425 g/cm 2 ).
  • the arm 22 is suspended from the polishing bowl edge and positioned on the side of the plate 20 in the path of its normal rotation which is caused by the rotation of plate 14.
  • the rotation of plate 14_ produces a rotation of the plate 20.
  • the surface of the parts 25 is continuously wetted with excess quantity of polishing slurry by flowing it through the pipe 32 with its restricted opening onto the surface 16 of rotating plate 14.
  • a parastolic pump 34 moves the slurry through the pipe 32. Excess slurry is splashed from the end of the rotating plate 14 and flows out of the excess slurry opening 12.
  • the citric acid-aqueous dispersion of silicon dioxide can be conveniently employed in the form of silica sols and silica gels having silicon dioxide particle sizes in the range of 1 to 500 nm (milli- microns), in concentrations of 6 to 16 weight percent silica.
  • the citric acid-aqueous dispersion of silicon dioxide or silicon dioxide slurry is required to have a pH in the range of about 7 to 9. It is preferable that the slurry have a pH slightly basic and of the order of 8.
  • the basic pH may be obtained by adding small quantities of citric acid solution of 80 grams/liter water to the dilute silicon dioxide slurry to produce the desired pH.
  • the slurry with the citric acid is stable for 48 hours without any gelling or precipitation. Slurries with other acids such as hydrochloric acid are stable for only short periods of time. At higher pH than 9 the surface will roughen, giving an orange-peel like effect. Lower pH polishing produces undesirable slow polishing rates.
  • the polishing time is also dependent upon the pre-polishing surface roughness condition.
  • the roughness of the pre-polishing surface is about 101.6 nm (peak to valley height).
  • the roughness of the pre-polishing surface depends upon the roughness of the substrate upon which the alumina is deposited, and upon the deposition method. That is the reason there is needed a highly perfect, polished substrate. The film is too thin for lapping, that is it cannot be abrasively polished for the same reason plus damage.
  • a chemical mechanical polishing process for polishing aluminum oxide operates very effectively to produce surface finishes of less than the order of 5.08 nm (0.2 micro inches) (peak to valley height). This measurement is actually the lower limit of the equipment so the surface finish is even better than that 5.08 nm.
  • the surface finish is measured by the conventional stylus method.
  • the chemical reaction is not fully understood but it appears that the citric acid water slurry has a reaction between the aluminum oxide and the water in the slurry to form an aluminum oxide- citric acid complex on the specimen surface which is in turn removed by the silicon dioxide slurry and polishing pad.
  • the apparent chemical reaction is:
  • the resulting polishing produces under these conditions no relief between the aluminum oxide grain boundaries and a highly perfect surface.
  • the solution was adjusted to a pH of 8 in this manner.
  • the polishing pressure used was 2.225 X 10 4 Pa.
  • the removal rate was 1.5 ⁇ m/hour.
  • the polished surface is rinsed in deionized water.
  • the polished surface finish (peak to valley) was 5.08 nm as determined by the conventional stylus method described in "Report on the Measurement of Surface Finish by Stylus Methods" by R. E. Reason, et al., published by the Rank Taylor Hobson Division Leicester, England 1944.
  • Amorphous aluminum oxide layers were prepared as in the Example 1. They were polished as described in Example 1 using pH of 9.5 and 11, the surfaces were visually unacceptable, due to pits and orange-peel. No removal rate data taken.

Claims (8)

1. Verfahren zum chemisch-mechanischen Polieren einer amorphen Aluminiumoxid-Oberfläche,
mit einem Substrat (8) mit einer Oberflächenschicht (9) aus dem Aluminiumoxid mit einer Stärke im Mikrometerbereich,
wobei die Aluminiumoxid-Oberfläche ständig mit einer Ueberschußmenge einer wässrigen Dispersion aus Zitronensäure und einem weichen Schleifmittel benetzt wird,
wobei die Aluminiumoxid-Oberfläche kontinuierlich mit einer festen Oberfläche (16) unter Anwendung von Druck abgewischt wird, während eine relative Bewegung zwischen der Aluminiumoxid-Oberfläche und der festen Oberfläche (16) aufrechterhalten wird, um das Produkt der Reaktion zwischen der Zitronensäure und dem Aluminiumoxid von den erhöhten Punkten der Aluminium-Oberfläche zu entfernen.
2. Verfahren nach Anspruch 1, bei dem der pH-Wert der wässrigen Lösung zwischen 7 und 9 liegt.
3. Verfahren nach Anspruch 1 oder 2, bei dem die Aluminiumoxid-Oberfläche eine aufgesprühte Schicht mit einer Stärke von 5 bis 8 Mikrometer ist.
4. Verfahren nach einem der Ansprüche 1 bis 3, bei dem die Aluminiumoxid-Oberfläche nach dem Polieren mit deionisiertem Wasser gespült wird.
5. Verfahren nach einem der Ansprüche 1 bis 4, bei dem die Aluminiumoxid-Oberfläche auf der Oberfläche eines Körpers aus einer fein gekörnten Mischung aus Aluminiumoxid und Titankarbid ist.
6. Verfahren nach einem der Ansprüche 1 bis 5, bei dem das weiche Schleifmaterial kolloidales Siliziumdioxid ist.
7. Verfahren nach Anspruch 6, bei dem der Siliziumdioxidanteil der Dispersion zwischen ca. 60 und 16 Gewichtsprozent liegt.
8. Verfahren nach einem der Ansprüche 1 bis 7, bei dem bei einem Druck von weniger als 4,25x 104 Pa (ca. 425 g/cm2) die Entfernungsgeschwindigkeit zwischen ungefähr 1,5 und 3 pm pro Stunde liegt.
EP19840101834 1983-03-10 1984-02-22 Verfahren zum Schleifen von gestaltlosem Aluminium-Oxyd Expired EP0121707B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US47412083A 1983-03-10 1983-03-10
US474120 1983-03-10

Publications (3)

Publication Number Publication Date
EP0121707A2 EP0121707A2 (de) 1984-10-17
EP0121707A3 EP0121707A3 (en) 1985-10-09
EP0121707B1 true EP0121707B1 (de) 1988-09-07

Family

ID=23882264

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19840101834 Expired EP0121707B1 (de) 1983-03-10 1984-02-22 Verfahren zum Schleifen von gestaltlosem Aluminium-Oxyd

Country Status (3)

Country Link
EP (1) EP0121707B1 (de)
JP (1) JPS5953317B2 (de)
DE (1) DE3473846D1 (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5527423A (en) * 1994-10-06 1996-06-18 Cabot Corporation Chemical mechanical polishing slurry for metal layers
US5582534A (en) * 1993-12-27 1996-12-10 Applied Materials, Inc. Orbital chemical mechanical polishing apparatus and method
US5643053A (en) * 1993-12-27 1997-07-01 Applied Materials, Inc. Chemical mechanical polishing apparatus with improved polishing control
US5650039A (en) * 1994-03-02 1997-07-22 Applied Materials, Inc. Chemical mechanical polishing apparatus with improved slurry distribution
US5858813A (en) * 1996-05-10 1999-01-12 Cabot Corporation Chemical mechanical polishing slurry for metal layers and films

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5232875A (en) * 1992-10-15 1993-08-03 Micron Technology, Inc. Method and apparatus for improving planarity of chemical-mechanical planarization operations
TW572980B (en) 2000-01-12 2004-01-21 Jsr Corp Aqueous dispersion for chemical mechanical polishing and chemical mechanical polishing process
US6910948B2 (en) 2001-09-27 2005-06-28 Nsk Ltd. Needle bearing and method for grinding bearing parts thereof

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1009884B (de) * 1955-07-08 1957-06-06 Vaw Ver Aluminium Werke Ag Verfahren zur Vorbehandlung von Werkstuecken aus Aluminium oder Aluminiumlegierungen zur Herstellung hochglaenzender, anodisch oxydierter Oberflaechen
CH356000A (de) * 1955-07-08 1961-07-31 Vaw Ver Aluminium Werke Ag Verfahren zur Herstellung haltbarer hochglänzender Oberflächen auf Werkstücken aus Aluminium oder einer Aluminiumlegierung
BE549314A (de) * 1955-07-08
US2940228A (en) * 1956-07-03 1960-06-14 Vaw Ver Aluminium Werke Ag Apparatus for polishing metals
US2942956A (en) * 1958-10-13 1960-06-28 Wyandotte Chemicals Corp Aluminum brightener compositions
US3053646A (en) * 1960-07-15 1962-09-11 Dow Chemical Co Grinding and polishing compositions and method of making same
DE1271288B (de) * 1965-02-23 1968-06-27 Monsanto Co Verfahren zum Polieren von Werkstoffen mittels eines Siliciumdioxyd enthaltenden Poliermittels
GB1109892A (en) * 1965-03-12 1968-04-18 Marshall Wolverhampton A new or improved metal polishing composition
US3906678A (en) * 1972-09-14 1975-09-23 Buehler Ltd Automatic specimen polishing machine and method
US3931696A (en) * 1974-03-04 1976-01-13 Veb Rathenower Optische Werke Device for making sections for specimens and specimen supports therefor
JPS6013788B2 (ja) * 1981-02-06 1985-04-09 住友特殊金属株式会社 単結晶フエライトの精密加工方法

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5582534A (en) * 1993-12-27 1996-12-10 Applied Materials, Inc. Orbital chemical mechanical polishing apparatus and method
US5643053A (en) * 1993-12-27 1997-07-01 Applied Materials, Inc. Chemical mechanical polishing apparatus with improved polishing control
US5899800A (en) * 1993-12-27 1999-05-04 Applied Materials, Inc. Chemical mechanical polishing apparatus with orbital polishing
US5913718A (en) * 1993-12-27 1999-06-22 Applied Materials, Inc. Head for a chemical mechanical polishing apparatus
US6019671A (en) * 1993-12-27 2000-02-01 Applied Materials, Inc. Carrier head for a chemical/mechanical polishing apparatus and method of polishing
US6267656B1 (en) 1993-12-27 2001-07-31 Applied Materials, Inc. Carrier head for a chemical mechanical polishing apparatus
US6503134B2 (en) 1993-12-27 2003-01-07 Applied Materials, Inc. Carrier head for a chemical mechanical polishing apparatus
US5650039A (en) * 1994-03-02 1997-07-22 Applied Materials, Inc. Chemical mechanical polishing apparatus with improved slurry distribution
US5527423A (en) * 1994-10-06 1996-06-18 Cabot Corporation Chemical mechanical polishing slurry for metal layers
US5858813A (en) * 1996-05-10 1999-01-12 Cabot Corporation Chemical mechanical polishing slurry for metal layers and films

Also Published As

Publication number Publication date
EP0121707A3 (en) 1985-10-09
JPS59170175A (ja) 1984-09-26
JPS5953317B2 (ja) 1984-12-24
EP0121707A2 (de) 1984-10-17
DE3473846D1 (en) 1988-10-13

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