WO2004036620A2 - Method for generating oxide layers on semiconductor substrates - Google Patents

Method for generating oxide layers on semiconductor substrates Download PDF

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Publication number
WO2004036620A2
WO2004036620A2 PCT/EP2003/011234 EP0311234W WO2004036620A2 WO 2004036620 A2 WO2004036620 A2 WO 2004036620A2 EP 0311234 W EP0311234 W EP 0311234W WO 2004036620 A2 WO2004036620 A2 WO 2004036620A2
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solution
ozone
temperature
oxide
use temperature
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PCT/EP2003/011234
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French (fr)
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WO2004036620A3 (en
Inventor
Jörg LEBERZAMMER
Reinhard Sellmer
Klaus Koller
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Sez Ag
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Priority to AU2003276093A priority Critical patent/AU2003276093A1/en
Publication of WO2004036620A2 publication Critical patent/WO2004036620A2/en
Publication of WO2004036620A3 publication Critical patent/WO2004036620A3/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
    • H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
    • H01L21/02244—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of a metallic layer
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
    • H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
    • H01L21/02178—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing aluminium, e.g. Al2O3
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
    • H01L21/02255—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by thermal treatment
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/02—Bonding areas; Manufacturing methods related thereto
    • H01L2224/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
    • H01L2224/04042—Bonding areas specifically adapted for wire connectors, e.g. wirebond pads
    • H—ELECTRICITY
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    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/44—Structure, shape, material or disposition of the wire connectors prior to the connecting process
    • H01L2224/45—Structure, shape, material or disposition of the wire connectors prior to the connecting process of an individual wire connector
    • H01L2224/45001—Core members of the connector
    • H01L2224/45099—Material
    • H01L2224/451—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof
    • H01L2224/45138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
    • H01L2224/45144—Gold (Au) as principal constituent
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    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L2224/85—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a wire connector
    • H01L2224/8536—Bonding interfaces of the semiconductor or solid state body
    • H01L2224/85375—Bonding interfaces of the semiconductor or solid state body having an external coating, e.g. protective bond-through coating
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    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/02—Bonding areas ; Manufacturing methods related thereto
    • H01L24/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
    • H01L24/05—Structure, shape, material or disposition of the bonding areas prior to the connecting process of an individual bonding area
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    • H01L2924/01—Chemical elements
    • H01L2924/01013—Aluminum [Al]
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    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/01—Chemical elements
    • H01L2924/01014—Silicon [Si]
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    • H01L2924/01072—Hafnium [Hf]
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    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/11—Device type
    • H01L2924/14—Integrated circuits

Definitions

  • the invention relates to a method for generating oxide layers on metal surfaces on semiconductor substrates.
  • Metal surfaces can be selected from the group aluminum, copper, silicon and an alloy thereof.
  • Oxide layers on metals might be generated on bonding pads, e.g. comprising aluminum (Al, AISi, AlSiCu). Such bonding pads are small areas on top of a semiconductor chip. These bonding pads are used in the production of integrated circuits for connection to wires (e.g. fine gold wires) which in turn are connected to the external circuit, other electronic or electrical components or are connected to a so called lead frame.
  • wires e.g. fine gold wires
  • Miyakawa [Improvement of Moisture Resistance by the New Surface Treatment of Aluminum Bonding Pads in LSI, T. Miyakawa et al., ISTFA '93, The 19 th International Symposium for Testing & Failure Analysis] proposed a method for forming a fine aluminum oxide film on aluminum bonding pads, in order to prevent corrosion due to moisture penetration. Miyakawa teaches immersion of a semiconductor wafer in an ozone solution in the last step of the wafer production process, to form an aluminum oxide film over the bonding pads.
  • a method for forming a protective oxide film is proposed.
  • the oxide layer is formed on bonding pads of a semiconductor chip, while the chip is in the form of wafer.
  • the wafer is exposed to ozone and ultraviolet (UV) radiation, so that excited oxygen, which is generated from the ozone by UV radiation, oxidizes metal atoms, for example aluminum atom of the aluminum bonding pads, to form a fine oxide film over the bonding pads.
  • UV radiation ultraviolet
  • the method for generating oxide layers on metal surfaces on semiconductor substrates comprises:
  • the liquid, in which ozone is dissolved is preferably an aqueous solution. Pure water is possible and deionized water is typically used. Depending on the selected temperature a desired oxide thickness can be achieved.
  • An additional advantage of the method according to the invention is that the solution will remove eventually organic and/or halogen contamination.
  • the point-of-use temperature is higher than 30°C. This leads to a good oxide layer giving sufficient protection to the metal layer underneath.
  • the forming of the solution by dissolving ozone in a liquid is carried out. at a dissolving temperature, which is lower than said point-of-use temperature.
  • a dissolving temperature which is lower than said point-of-use temperature.
  • Yet another embodiment of the method includes a step wherein the metal surface is pretreated with an oxide-removing agent before it is treated with the solution.
  • the pretreatment with oxide-removing agent is useful if the metal surface has been exposed to ambient atmosphere for a longer time and the metal (e.g. Al) tends to form native oxide together with oxygen coming from air.
  • the metal e.g. Al
  • the point-of-use temperature is achieved by heating the solution after dissolving the ozone or by applying heat energy to the backside of semiconductor substrate (e.g. through a heated fluid). Further details of the invention follow from the example below.
  • a semiconductor wafer having aluminum bonding pads exposed is placed on a spin chuck as described in EP1170782A2.
  • the wafer is pretreated with DHF at ambient temperature for about 5 seconds. While rotating the spin chuck and the wafer thereon the wafer is heated by supplying deionized water onto the backside of the wafer.
  • the backside shall be defined as the side of the wafer not having bonding pads exposed to be treated.
  • the selected temperature is 50°C.
  • the spin speed is 50 to 3000 rpm, preferably 200 to 1000 rpm.
  • Deionized water (ambient temperature) is fed into an ozone module where ozone is dissolved in the water through a membrane to achieve an aqueous solution with a concentration of about 50ppm ozone.
  • the ozone is being generated from oxygen treated with electrical discharge. .
  • the solution is heated to a temperature of 50°C in line immediately before dispensing the solution onto the wafer's front surface.
  • the wafer is treated for 4,5 minutes. This results in an aluminum oxide layer of a thickness of 20 nm. It has been seen that a treatment time of even five minutes does not result in a significantly higher thickness. - - • -
  • Fig. 1 shows a diagram of the aluminum oxide thickness d as a function of the treating time t at two different treating temperatures T (23°C and 50°C). This shows for instance that at 50°C with a treatment of only 60 seconds an oxide thickness of 12 nm can be achieved.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
  • Formation Of Insulating Films (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

A method is disclosed for generating oxide layers on metal surfaces on semiconductor substrates. The method comprising forming a solution by dissolving ozone in a liquid, and reacting the said solution with said surface at a selected point-of-use temperature, which is higher than ambient temperature.

Description

Method for generating oxide layers surfaces on semiconductor substrates
The invention relates to a method for generating oxide layers on metal surfaces on semiconductor substrates. Metal surfaces can be selected from the group aluminum, copper, silicon and an alloy thereof. Oxide layers on metals might be generated on bonding pads, e.g. comprising aluminum (Al, AISi, AlSiCu). Such bonding pads are small areas on top of a semiconductor chip. These bonding pads are used in the production of integrated circuits for connection to wires (e.g. fine gold wires) which in turn are connected to the external circuit, other electronic or electrical components or are connected to a so called lead frame.
When dicing the wafers to achieve single dice the wafers are sawed. During sawing process particles (sawing mud) might adhere on the bonding pads. Such particles can lead to bonding problems. To make it easier to clean the bonding pads on the chips after dicing, oxide layers on metal surfaces are used to protect the metal surface. Additional, the bond pad surfaces are contaminated with halogens and organic materials from former process steps, which can degrade the bond connection and will reduce the product lifetime.
Miyakawa [Improvement of Moisture Resistance by the New Surface Treatment of Aluminum Bonding Pads in LSI, T. Miyakawa et al., ISTFA '93, The 19th International Symposium for Testing & Failure Analysis] proposed a method for forming a fine aluminum oxide film on aluminum bonding pads, in order to prevent corrosion due to moisture penetration. Miyakawa teaches immersion of a semiconductor wafer in an ozone solution in the last step of the wafer production process, to form an aluminum oxide film over the bonding pads.
To get an oxide layer of higher thickness in US05595934A a method for forming a protective oxide film (layer) is proposed. The oxide layer is formed on bonding pads of a semiconductor chip, while the chip is in the form of wafer. The wafer is exposed to ozone and ultraviolet (UV) radiation, so that excited oxygen, which is generated from the ozone by UV radiation, oxidizes metal atoms, for example aluminum atom of the aluminum bonding pads, to form a fine oxide film over the bonding pads. This film provides protection from water and/or ions, which would otherwise cause corrosion of the bonding pads.
It is an object of the invention to provide a method for generating oxide layers on metal layers on semiconductor substrates, in which metal layers are covered with an oxide layer in a simple and effective way and to achieve an oxide layer of sufficient high thickness.
It has been tested to generate oxide layers of sufficient thickness by supplying water with therein-dissolved ozone similar to Miyakawa's process. At room temperature no satisfying results could be achieved - the thickness was below 5 nm. Therefore temperature was lowered in order to dissolve a higher amount of ozone in the water but the result did not become better. The thickness of the oxide layer was independent of the process time. Even ten minutes or more did not lead to a significant higher thickness than a one-minute treatment time.
By raising the point-of-use temperature after dissolving a sufficient high amount of ozone in the water, it was surprisingly seen that the thickness of the oxide layer had become even higher as could be seen by alternative methods described in prior art.
It was found out that neither the concentration of ozone in the solution nor the time factor had that much of an impact as raising the temperature had. By raising the temperature from ambient temperature to about 40°C the thickness of the oxide layer increased from below 6 nm to above 10 nm. This does not seem to be because the reaction speed does increase by raising the temperature because even a very long treatment (over ten minutes instead of one minute) of the metal surface with ozonized solution did not lead to a significant higher oxide thickness.
According to the invention the method for generating oxide layers on metal surfaces on semiconductor substrates comprises:
• forming a solution by dissolving ozone in a liquid, and
• reacting said solution with said surface at a selected point-of-use temperature, which is higher than ambient temperature. The liquid, in which ozone is dissolved, is preferably an aqueous solution. Pure water is possible and deionized water is typically used. Depending on the selected temperature a desired oxide thickness can be achieved.
An additional advantage of the method according to the invention is that the solution will remove eventually organic and/or halogen contamination.
In one embodiment the point-of-use temperature is higher than 30°C. This leads to a good oxide layer giving sufficient protection to the metal layer underneath.
There are basically two different possibilities to apply the ozonized solution to a substrate. One is immersing the substrate into the solution. The other one is dispensing (or supplying) the solution onto the wafer. Whereas both ways of treatment are possible the latter is preferred. This gives the advantage to select the treatment temperature more precisely which leads to better uniformity.
In another embodiment the forming of the solution by dissolving ozone in a liquid is carried out. at a dissolving temperature, which is lower than said point-of-use temperature. This gives the advantage to have a higher ozone concentration in the solution. The higher point of use temperature could thus lead to a supersaturated solution and ozone tends to leave the solution, which leads to an even higher reactivity of ozone at the point-of-use.
Yet another embodiment of the method includes a step wherein the metal surface is pretreated with an oxide-removing agent before it is treated with the solution. This leads to a blank oxide-free surface and therefore the lack of a passivation layer which otherwise could prevent the generating of a smooth oxide-layer. Such an oxide- removing agent could be an aqueous solution of hydro fluoric acid (diluted hydro fluoric acid = DHF), preferably with a concentration of 0,1% to 5% HF per weight.
The pretreatment with oxide-removing agent is useful if the metal surface has been exposed to ambient atmosphere for a longer time and the metal (e.g. Al) tends to form native oxide together with oxygen coming from air.
The point-of-use temperature is achieved by heating the solution after dissolving the ozone or by applying heat energy to the backside of semiconductor substrate (e.g. through a heated fluid). Further details of the invention follow from the example below.
A semiconductor wafer having aluminum bonding pads exposed is placed on a spin chuck as described in EP1170782A2.
The wafer is pretreated with DHF at ambient temperature for about 5 seconds. While rotating the spin chuck and the wafer thereon the wafer is heated by supplying deionized water onto the backside of the wafer. The backside shall be defined as the side of the wafer not having bonding pads exposed to be treated.
The selected temperature (point-of-use temperature) is 50°C. The spin speed is 50 to 3000 rpm, preferably 200 to 1000 rpm.
Deionized water (ambient temperature) is fed into an ozone module where ozone is dissolved in the water through a membrane to achieve an aqueous solution with a concentration of about 50ppm ozone. The ozone is being generated from oxygen treated with electrical discharge. .
The solution is heated to a temperature of 50°C in line immediately before dispensing the solution onto the wafer's front surface.
To preheat the wafer to the same temperature as the temperature of the solution brings the advantage of better uniformity across the wafer.
The wafer is treated for 4,5 minutes. This results in an aluminum oxide layer of a thickness of 20 nm. It has been seen that a treatment time of even five minutes does not result in a significantly higher thickness. - - • -
In another example a blank metal surface is exposed and therefore the pretreatment to remove eventual native oxide could be left out.
Fig. 1 shows a diagram of the aluminum oxide thickness d as a function of the treating time t at two different treating temperatures T (23°C and 50°C). This shows for instance that at 50°C with a treatment of only 60 seconds an oxide thickness of 12 nm can be achieved.

Claims

Claims:
1. Method for generating oxide layers on metal surfaces on semiconductor substrates comprising:
•. forming a solution by dissolving ozone in a liquid, and • reacting the said solution with said surface at a selected point-of-use temperature, which is higher than ambient temperature.
2. Method as claimed in claim 1 wherein the point-of-use temperature is higher than 30°C.
3. Method as claimed in claim 1 wherein the sofution is applied onto the metal surface on semiconductor substrate by dispensing the solution onto the metal surface.
4. Method as claimed in claim 1 wherein forming of the solution by dissolving ozone in a liquid at a dissolving temperature which is lower than said point-of-use temperature.
5. Method as claimed in claim 1 wherein the metal surface is pretreated with an oxide-removing agent before it is treated with the solution.
6. Method as claimed in claim 1 wherein the surface is a bonding pad comprising aluminum.
7. Method as claimed in claim 1 wherein the point-of-use temperature is achieved by heating the solution after dissolving the ozone.
8. Method as claimed in claim ϊ wherein the pbint-όf-use temperature is achieved by applying heat energy to the backside of semiconductor substrate.
9. Method as claimed in claim 8 wherein the point-of-use temperature is achieved by applying heated fluid to the backside of semiconductor substrate.
10. Method as claimed in claim 1 wherein the thickness of said oxide layer is more than 5 nm.
PCT/EP2003/011234 2002-10-14 2003-10-10 Method for generating oxide layers on semiconductor substrates WO2004036620A2 (en)

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US6240933B1 (en) * 1997-05-09 2001-06-05 Semitool, Inc. Methods for cleaning semiconductor surfaces
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WO2003090792A2 (en) * 2002-04-26 2003-11-06 Phifer Smith Corporation Method and apparatus for treating a substrate with an ozone-solvent solution iii
US20040067639A1 (en) * 2002-10-05 2004-04-08 Taiwan Semiconductor Manufacturing Co., Ltd. Method for forming low thermal budget sacrificial oxides

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US5565378A (en) * 1992-02-17 1996-10-15 Mitsubishi Denki Kabushiki Kaisha Process of passivating a semiconductor device bonding pad by immersion in O2 or O3 solution
EP0701275A2 (en) * 1994-08-26 1996-03-13 MEMC Electronic Materials, Inc. Pre-thermal treatment cleaning process
US6240933B1 (en) * 1997-05-09 2001-06-05 Semitool, Inc. Methods for cleaning semiconductor surfaces
US20020020436A1 (en) * 1997-05-09 2002-02-21 Bergman Eric J. Process and apparatus for treating a workpiece with steam and ozone
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