CN108115592A - It is used to prepare chemical-mechanical planarization（CMP）The aerosol method of polishing pad - Google Patents
It is used to prepare chemical-mechanical planarization（CMP）The aerosol method of polishing pad Download PDFInfo
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- CN108115592A CN108115592A CN201711227509.XA CN201711227509A CN108115592A CN 108115592 A CN108115592 A CN 108115592A CN 201711227509 A CN201711227509 A CN 201711227509A CN 108115592 A CN108115592 A CN 108115592A
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- reaction mixture
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/16—Making expandable particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D13/00—Wheels having flexibly-acting working parts, e.g. buffing wheels; Mountings therefor
-
- 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
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
- B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
- B29C67/24—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 characterised by the choice of material
- B29C67/246—Moulding high reactive monomers or prepolymers, e.g. by reaction injection moulding [RIM], liquid injection moulding [LIM]
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3237—Polyamines aromatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The method that offer of the present invention prepares CMP pad or layer, therefore, the method includes introduces two kinds without solvent and generally water-free component into the static mixer for having nozzle in downstream respectively, liquid polyhydric alkoxide component with temperature T1 and the liquid isocyanate component with temperature T2 under the low gauge pressure of each comfortable 5 to 120kPa (1 arrives 14psi), the liquid polyhydric alkoxide component includes one or more polyalcohols, amine hardener；And the liquid isocyanate component includes one or more polyisocyanate or isocyanate-terminated carbamate prepolymer；Described two components are mixed in the static mixer and form reaction mixture, the material flow of the reaction mixture is discharged to from the nozzle on the open type die substrate with carbamate release surface, and is formed by curing porosity polyurethanes reaction product.
Description
The present invention relates to manufacture porosity polyurethanes (PU) elastomer articles and chemical-mechanical planarization (CMP) to throw
The method of light pad, the mixing and under ambient pressure from its discharge without solvent and generally not included in static mixer
It aqueous two component reaction mixtures and is discharged on mold, and is formed by curing the pad, wherein in the method, not having
Gas injection and the reaction mixture are generally free of foaming agent in the oriented reaction mixture.
Include addition porous polymerizing filler for manufacturing the known method of porosity CMP pad, such as be added to
In the polymeric matrices of molding, mechanical foaming is carried out to gas/polyurethanes (PU) mixture for curing to intercept and capture bubble；Add
Add foaming agent or form hole from the gas physically or chemically generated using water；And to overcritical (SC) fluid (such as SC-
CO2) saturation polymer carry out fast decompression.However, in any this kind of method, the gas of a large amount of volumes is introduced into pulvilliform
Needs adjusted before gas is included are generated in resulting mixture, and improve during processing with after processing
Ventilation and effluent processing requirement.Being generated in pulvilliform resulting mixture or introduce gas may not to form the known method of hole
Uniform pores distribution or homogeneous filling mold can be formed to manufacture CMP pad.In addition, air or gas are introduced into this kind of use
In manufacture CMP pad reaction mixture in or this kind of for manufacture CMP pad reaction mixture in generate gas
Two from spraying device kinds may be caused mutually to flow, this can lack uniformity, make liquid flow and gas at ejection end or nozzle
Replace between body stream, so as to which heterogeneous material be caused to discharge and striped is generated in products therefrom.
The U.S. Patent No. 8,314,029 for giving uncommon Ross (Hirose) et al. discloses the side of manufacture CMP pad
Method forms composition and from single outlet into plane materiel comprising carbamate is disperseed by mechanical foaming manufacturing cell
Center portion point persistently discharges composition, wherein can discharge polyurethanes from it in longitudinal feed-in plane materiel, adjusts on plane materiel
Carbamate forms the thickness of composition, and does not apply extra load, that is, solidification composition filling to composition.Mechanical foaming will
Nullvalent gas is introduced into reaction mixture.
The present inventor seek solve provide for manufacture with improve homogeneity chemical mechanical polishing pads application or
Spray method.
The content of the invention
1. the method for according to the present invention, preparing chemical-mechanical planarization (CMP) polishing pad is included respectively in downstream end
There is two kinds of introducing in the static mixer of nozzle to arrive 200kPa without solvent and generally water-free component, each comfortable 100
Or preferably 100 to the liquid polyhydric alkoxide component with temperature T1 and the liquid isocyanide with temperature T2 under 150kPa absolute pressures
Acid esters component, forms the flowing by mixer, and the liquid polyhydric alkoxide component includes one or more polyalcohols, amine curing
Agent, preferably aromatic diamine, and various trace elements are additionally comprised, such as polymeric microspheres bead；And the liquid
Isocyanate component includes one or more polyisocyanate or isocyanate-terminated carbamate prepolymer, preferably fragrant
The carbamate prepolymer of fragrant adoption isocyanates or aromatic isocyanate sealing end；By the total solid of the reaction mixture
Weight meter, at least one component, preferably described liquid polyhydric alkoxide component are arrived comprising at most 2.0wt.% or preferably 0.1
The nonionic surfactant of the sufficient amount of 1.0wt.%, preferably organopolysiloxane -co- polyethet surfactant are to promote
Hole is stablized, and described two components are mixed in the static mixer and form reaction mixture, by the reaction mixture
Material flow is discharged to the die substrate with carbamate release surface, such as polytetrafluoroethylene (PTFE) from the nozzle, preferably has
There is the open type mold of concave surface form, the configuration of surface fills the mold shape with the reaction mixture of the application
Into the required groove pattern of CMP pad, and in environment temperature to 130 DEG C or preferably in environment temperature to curing at 100 DEG C
Form porosity poly- amino first of the density in the range of 0.6gm/cc to 1gm/cc or preferably 0.75gm/cc to 0.95gm/cc
Acid esters reaction product.
2. according to the method for the manufacture CMP pad of the present invention as illustrated in above-mentioned item item 1, wherein the nozzle fills
The atomizing air inlets or air blast lid around the nozzle exterior are had, thus air stream flows through the point of the nozzle
End, then flows axially through along the material flow of the discharge of the reaction mixture.
3. according to the method for manufacturing CMP pad for the present invention that such as any one of above-mentioned item item 1 or 2 is illustrated, wherein
Foaming agent of the reaction mixture without addition, the chemically or physically foaming agent including being free of addition.
4. the method for manufacturing CMP pad of the invention illustrated according to such as any one of above-mentioned item item 1,2 or 3,
Described in reaction mixture at curing temperatures have 2 to 300 seconds or preferably 5 to 60 seconds or the more preferably glue of 5 to 45 seconds
The solidifying time.
5. the method for manufacturing CMP pad of the invention illustrated according to such as any one of above-mentioned item item 1,2,3 or 4,
Wherein when every in the liquid polyhydric alkoxide component and the liquid isocyanate component of temperature T2 that temperature T1 is introduced into static mixer
At one, each there is 1 to 1000cP or preferably 100 viscosity for arriving 500cP, wherein each in T1 and T2 is at 10 DEG C
In the range of to 80 DEG C or in the range of preferably 15 to 40 DEG C or more preferably environment temperature.
6. according to the method for manufacturing CMP pad for the present invention that such as above-mentioned item item 5 is illustrated, in addition wherein, liquid is more
Each in first alkoxide component and liquid isocyanate component is individually preheating to temperature before static mixer is introduced into
T1 and/or T2.
7. according to the side for manufacturing CMP pad for the present invention that such as any one of above-mentioned item item 1,2,3,4,5 or 6 is illustrated
Method, wherein liquid polyhydric alkoxide component additionally comprise one of trace element, such as polymeric microspheres or at most 3000ppm or excellent
Selection of land at most 1500ppm water improves pad porosity.
8. according to the side for manufacturing CMP pad for the present invention that such as any one of item item 1,2,3,4,5,6 or 7 is illustrated
Method, wherein reaction mixture are without solvent and generally not aqueous.
9. according to the side for being used to manufacture CMP pad of the present invention as illustrated in any of the above described first preceding article item 1 to 8
Method is included first in environment temperature wherein curing the reaction mixture to curing 1 to 30 minutes or preferably 30 at 130 DEG C
Second, to the period of 5 minutes, polyurethanes reaction product was removed from the mold；Then finally at 60 DEG C to 130
Cure at a temperature of DEG C 1 minute to 16 when small or preferably 5 minutes to 15 minutes period formed porosity article.
10. according to such as the method for the present invention in above-mentioned item item 10, wherein formed the polishing pad be further contained in it is described
Subpad layer is stacked on the bottom side of porosity article, such as polymer impregnated nonwoven or porosity or non-porous polymer sheets so that institute
The molded surface for stating porosity article forms the top surface of CMP pad.
11. according to the method for the present invention such as any one of above-mentioned item item 1 to 10, wherein the material by the reaction mixture
Stream is discharged on mold, comprising mold described in overspray, is subsequently cured the reaction mixture therefore applied and is formed poly- amino first
Acid esters reaction product removes the polyurethanes reaction product from the mold and then by the polyurethane
The periphery of ester reaction product is punched or cut out the required diameter of CMP pad.
12. according to the method for the present invention such as any one of above-mentioned item item 1 to 11, wherein static mixer, it is included under it
The nozzle at end is swum, is consolidated by the mechanical actuator original place that can be now parallel to move in the plane on the surface of open type mold in fact
It holds, the mechanical actuator is for example with the programmable electronic actuator that can realize the mobile mechanical linkage of programming, it is preferable that
With four armshafts for being capable of XY axial movements or it is capable of the automatic machines of XYZ axial movements and six armshafts in rotary moving.For this
The purpose of specification, unless otherwise specifically stated, otherwise composite is all represented with wt%.
Unless otherwise instructed, otherwise temperature and pressure condition is environment temperature and normal pressure (101kPa).
Unless otherwise instructed, otherwise any term containing round parentheses can alternatively refer to whole terms, just as circle includes
It number is not present and term does not have round parentheses the same and the combination of each alternative solution.Therefore, term " (poly-) isocyanates "
Refer to isocyanates, polyisocyanate or its mixture.
All scopes are all inclusive and can be combined.For example, " 50 arrive 3000cp or 100cp or bigger to term
Scope " will be including each in 50cp to 100cp, 50cp to 3000cp and 100cp to 3000cp.
Unless otherwise instructed, otherwise as used herein, " average molecular weight " of term polymer refers to oozing by gel
Saturating chromatography measured to specifying or if non-designated known appropriate criteria product, as being directed to the poly(ethylene glycol) of polyalcohol
As a result.
As used herein, term " gelling time " means the result by following acquisition：It is for example being set at about 80 DEG C
Be scheduled under 1000rpm VM-2500 vortex laboratory blender (StateMix Ltd., Canadian Winnipeg (Winnipeg,
Canada the given reaction mixture of mixing 30 seconds in))；It sets the timer to 0 and opens timer；Pour the mixture into aluminium
In cup；Cup is put into gelling timer (the Gardco Hot Pot being set at 65 DEG CTMBe gelled timer, Florida State
Ripple Barnes ＆ Noble than strange Borrow N Gardners Co., Ltd (Paul N.Gardner Company, Inc., Pompano Beach,
FL in electric food warmer))；Mixture, which is stirred to react, with the wire stirrer under 20RPM and records wire stirrer stops at sample
Gelling time when being moved in product.
As used herein, term " ASTM " refers to Xikang She Huoken ASTM international organizations of Pennsylvania
The publication of (ASTM International, West Conshohocken, PA).
As used herein, term " polyisocyanate " means any containing different containing two or more isocyanate group
The molecule of cyanic acid ester group.
As used herein, term " polyurethanes " refers to difunctionality or the polymerizate of polyfunctional isocyanate,
Such as polyethers urea, poly-isocyanurate, polyurethanes, polyureas, polyurethane-urea, its copolymer and its mixture.
As used herein, term " reaction mixture " includes any non-reacted additive, such as trace element and reduction CMP
Polyurethanes reaction product in polishing pad is according to any additive of the hardness of ASTM D2240-15 (2015).
As used herein, " stoichiometry " of term reaction mixture refers to that (free OH+ dissociates in the reactive mixture
NH2Group) molar equivalent and dissociateive NCO group molar equivalent ratio.
As used herein, term " SG " or " proportion " refer to the density and phase of polishing pad manufactured according to the present invention or layer
The ratio of the density of synthermal lower water.
As used herein, term " solid " refers to being retained in any in the polyurethanes reaction product of the present invention
Material；Therefore, solid is included in nonvolatile reactive and non-volatile additive during curing.Solid does not include water and volatility
Solvent.
As used herein, unless otherwise instructed, otherwise term " generally not aqueous " means given combination object with low
There is adding less than 2000ppm in the addition water of 2,000ppm or preferably no added water and into the material in composition
Add water or preferably no added water.The reaction mixture of " generally not aqueous " can be arrived comprising present in raw material 50
Water in the range of 2000ppm can include the reaction water formed in condensation reaction or from the ambient water for using reaction mixture
The steam divided.
As used herein, term means given combination object without addition chemically or physically " generally without foaming agent "
Foaming agent.Foaming agent does not include water.The air-flow being not considered as through nozzle is a part for given combination object.
As used herein, unless otherwise instructed, otherwise term " viscosity " refers to such as putting down in the 50mm with 100 μm of spacing
In andante geometry using measured by the rheometer for the steady shear for being set in 1 radian per second at a given temperature in pure
The viscosity of the given material of form (100%).
As used herein, term " wt.% " represents weight percent.
Description of the drawings
Fig. 1 is for the description of the perspective view of the equipment of the method for the present invention.
The present invention realizes a kind of be used for from two component reaction mixtures preparation porosity polyurethanes CMP pad
Simple spray applications method, without using foaming agent and at the same time by liquid reaction mixture after mixer outlet discharge
Aerosol is generated to avoid gas injection.The only gas used in the method for the present invention is surrounding air.Form fluid reaction
It mixture and is applied to the pressure of open type mold and is at most 200kPa (in static mixer inlet) to environmental pressure
In the range of (at static mixer lower exit).The method of the present invention is by making when being discharged in open type mold and afterwards
Reaction mixture material flow retains surrounding air to form hole.Therefore, when no trace element or polymeric microspheres exist
When, the air of embedding forms hole, and average pore size is at 5 to 100 μm or preferably in 10 to 40 μ ms.The method of the present invention
Low pressure makes that in two component reaction mixtures trace element can be included or the hole being easily destroyed forms additive.It is in addition, of the invention
The simple and open type mold property of method allows to using extremely fast curing reaction mixture, such as gelling time 5 to 45 seconds
Those or the gelling time at most large range of reaction mixture for reacting slower of 300 seconds.In addition, the method for the present invention
Combining for mixing intensity or pressure and the fogging degree of reaction mixture that is generated during discharge is released, is thus allowed by fully mixing
It is more than 20 μm or even more than 40 μm of molded articles or CMP pad that the reaction mixture of conjunction, which forms average pore size,.Finally, originally
Inventive method and the low viscosity of two component reaction mixtures realize together the filling of fabulous mold and die surface in molded articles or
Duplication in CMP pad.Equipment used is included through two conduits in the method for the present invention, through such as peristaltic pump or positive row
It measures the pump feed-in such as piston pump and there is the simple static mixer of the downstream spray nozzle equipped with atomizing air capping, described two
One for liquid isocyanate component in a conduit and another is for liquid polyhydric alkoxide component.Static mixer is at most
200kPa (in static mixer inlet) is to operating under environmental pressure (at static mixer outlet).
The spray nozzle of the present invention can be the simple tapers nozzle that atomizing space source of the gas is equipped with around nozzle exterior, described
Atomizing space source of the gas such as air blast lid or atomizing air inlets.Air blast lid is placed in nozzle base, and and nozzle
The outside of base portion forms annular gap together, and surrounding air is made to flow to the tip of nozzle, then along the reaction mixture discharged
Material flow is axially flowed and flowed on substrate.Air blast lid and nozzle is suitble to be obtained from the promise letter of Rhode Island Providence
EFD.(Nordson EFD.,Providence,RI)。
It is arrived by the air flow rate of air blast lid or atomizing air inlets 20 to 180L/min or preferably 30
In 150L/min flow rate ranges.
A kind of suitable equipment includes two parts：From holding tank to the liquid polyol of static mixer feed-in control ratio
The metering pump of component and liquid isocyanate component and being equipped with rouses the air that reaction mixture blends and is sprayed on substrate
The static mixer at general mood solation tip.
Two conduits into the static mixer in present device can include metering or transmission system, such as a pair of of gas
The positive displacement piston pump of dynamic driving, each by liquid polyhydric alkoxide component or liquid isocyanate component through a succession of accessory and pipeline
It applies and is fitted on static mixer.A/B ratios are controlled by the lever arm for the relative motion for mechanically changing two piston pumps.This
The example of kind equipment can be used as PosiratioTMThe mini PRM instrument (Graco of Minneapolis, Minnesota
(Graco, Minneapolis, MN)) it is commercially available.Another example is two laboratory level peristaltic pumps, is transferred respectively to static mixer
Liquid isocyanate component and liquid polyhydric alkoxide component.
As shown in fig. 1, static mixer (12) tool is each respectively used to liquid there are two fluid inlet conduit (16 and 18)
Body isocyanate component and liquid polyhydric alkoxide component.Static mixer (12) has nozzle (20) in downstream, and equipment is free
Enraged windshield (14) helps from nozzle (20) atomisation.
The reaction mixture of the present invention does not include solvent and not comprising addition water, but can be by the at most water of 2000ppm
It is added in liquid polyhydric alkoxide component that hole is promoted to be formed.
The mold of the present invention is made or is lined with non-adhesive material by non-adhesive materials such as such as polytetrafluoroethylene (PTFE).Preferably, mold
It is processed to be formed in the form of concave surface so that the polyurethanes reaction product of gained molding has desired channel.
Preferably, the substrate in the method for the present invention is mold, wherein manufactured CMP pad will be directly incorporated into slot figure
Case.For example, mold can have concave surface form, and the configuration of surface fills mold with the reaction mixture of application
Form the groove pattern of pad.
The liquid isocyanate component of the present invention can include diisocyanate, triisocyanate, chlorinated isocyanurates, isocyanide
Acid esters sealing end carbamate prepolymer or its mixture in any one.Preferably, liquid isocyanate component includes virtue
Fragrant adoption isocyanates, the aromatic diisocyanate such as selected from the following：Methyl diphenylene diisocyanate (MDI)；
Toluene di-isocyanate(TDI) (TDI)；Naphthalene diisocyanate (NDI)；Paraphenylene diisocyanate (PPDI)；Ortho-toluidine diisocyanate
(TODI)；Modified methyl diphenylene diisocyanate, methyl diphenylene diisocyanate, urea groups such as Carbodiimide-Modified
The ester modified methyl diphenylene diisocyanate of formic acid, biuret modified methyl diphenylene diisocyanate；Aromatic series isocyanide
Urate, such as the chlorinated isocyanurates of MDI；Linear isocyanate-terminated carbamate prepolymer, such as MDI or MDI dimerization
The linear isocyanate-terminated carbamate prepolymer of body and one or more isocyanate extenders.
Suitable isocyanate extender is ethylene glycol；1,2- propylene glycol；1,3- propylene glycol；1,2- butanediols；1,3- fourths two
Alcohol；2- methyl-1,3-propanediols；1,4- butanediols；Neopentyl glycol；1,5- pentanediols；3- methyl-1s, 5- pentanediols；1,6- oneself
Glycol；Diethylene glycol；Dipropylene glycol；Tripropylene glycol and its mixture.
The liquid isocyanate component of the present invention can have based on the total solid weight of aromatic isocyanate component,
High unreacted isocyanates (NCO) concentration of 10wt.% to 40wt.% or preferably 15wt.% to 35wt.%.
Isocyanate-terminated carbamate prepolymer is suitble to preferably to have less than 0.1wt% to dissociate diisocyanate
The isocyanate-terminated carbamate prepolymer of toluene ester (TDI) content of monomer.
The liquid polyhydric alkoxide component of the present invention can be that any one or more of glycol with terminal hydroxyl or polyethers are more
First alcohol, such as glycol, polyalcohol, polyalcohol glycol, its copolymer and its mixture.Preferably, one or more polyalcohol choosings
From polyether polyol (such as poly- (oxygroup tetramethylene) glycol, poly- (oxygroup propylidene) glycol and its mixture)；Poly- carbonic acid
Ester polyol；Polyester polyol；Polycaprolactone polyol；Its mixture；And it is selected from the following with one or more
The mixture of low molecular weight polyols：Ethylene glycol；1,2- propylene glycol；1,3- propylene glycol；1,2- butanediols；1,3 butylene glycol；2-
Methyl-1,3-propanediol；1,4- butanediols；Neopentyl glycol；1,5- pentanediols；3- methyl-1s, 5- pentanediols；1,6-HD；
Diethylene glycol；Dipropylene glycol；And tripropylene glycol.
It is highly preferred that one or more polyalcohols of the liquid polyhydric alkoxide component of the present invention are selected from the following：Poly- four is sub-
Ether glycol (PTMEG)；Containing ester polyol (such as adipic acid second diester, adipic acid fourth diester)；Polypropylene ether glycol
(PPG)；Polycaprolactone polyol；Its copolymer；And its mixture.
Suitable polyalcohol can include number average molecular weight MNIt is 500 to 10,000 polyalcohol.Preferably, it is used more
The number average molecular weight M of first alcoholNIt is 500 to 6,000 or more preferably 500 to 4,000；Most preferably 1,000 to 2,000.
This kind of high molecular weight polyols preferably per molecule has average 3 to 10 hydroxyls.It is highly preferred that high molecular weight polyols used
Per molecule has average four to eight or more preferably five to seven or most preferably six hydroxyls.Height containing 6 hydroxyls
The example of molecujar weight polyol is the poly- propoxyl group -co- ethyoxyl sugar alcohol for having ethyoxyl hydroxyl, such as D-sorbite.
The amine hardener of the present invention is that have one or more or the preferably amine of two or more amidos or polynary
Amine or preferably aromatic polyamine such as have the aromatic diamine and aromatic polyamine of 3 amidos.It is it is highly preferred that fragrant
Race's polyamine is selected from the group being made of the following：Dimethylthiotoluenediamine；Two-P aminobenzoates of propylene glycol；It is poly-
Two-P aminobenzoates of tetrahydrofuran；PolyTHF list-P aminobenzoates；Polypropylene oxide two-p-aminophenyl first
Acid esters；Polypropylene oxide list-P aminobenzoates；Double (2- aminobenzene-thios) ethane of 1,2-；Toluenediamine, such as diethyl first
Phenylenediamine, 5- tertiary butyl -2,4- toluenediamines, 3- tertiary butyl -2,6- toluenediamines, 5- tertiary pentyl -2,4- toluenediamines, uncle 3-
Amyl -2,6- toluenediamine, 5- tertiary pentyl -2,4- chloromethane phenylenediamines and 3- tertiary pentyl -2,6- chloromethane phenylenediamines；Methylene two
Aniline, such as 4,4'- methylene-bis--aniline；Isophorone diamine；1,2- diaminocyclohexanes；Double (4- aminocyclohexyls) first
Alkane, 4,4'- diamino diphenyl sulfones；M-phenylene diamine (MPD)；Dimethylphenylene diamine；1,3- is double (aminomethyl hexamethylene)；And its mixing
Object, preferably dimethylthiotoluenediamine.
In general, amine (NH in reaction mixture2) base total mole number and hydroxyl (OH) total mole number summation ratio
The stoichiometry of the total mole number of unreacted isocyanates (NCO) base is in 0.8 in reaction mixture:1.0 to 1.1:1.0
Or in the range of preferably 0.95 to 1.05.
The CMP pad of the present invention can further include various trace elements, preferably be dispersed in entire throwing
In photosphere.Preferably, trace element selected from hollow core polymeric material, gather by the hollow core as polymeric microspheres, liquid are filled
Condensation material, such as the polymeric microspheres that fluid is filled, water-soluble material and insoluble phase material (such as mineral oil).It is it is highly preferred that micro-
Secondary element is selected from hollow core polymeric material.Preferably, micro- weight mean diameter is less than 150 μm or more preferably
Less than 100 μm；Most preferably 5 to 50 μm.Preferably, the various trace elements, which include, has polyacrylonitrile or polyacrylonitrile
Polymeric microspheres (such as the Expancel of the shell wall of copolymerTMBead, the Akzo Nobel from Amsterdam, the Netherlands
Company (Akzo Nobel, Amsterdam, Netherlands)).When in use, the amount of trace element can be in CMP pad
Or it generates 0.1 in polishing layer and is arrived to 50vol.% porositys or preferably 5 in the range of the amount needed for 35vol.% porositys.
Term " porosity " refers to the volumetric concentration of trace element divided by the volume of gained CMP pad or layer.
The chemical mechanical polishing pads being prepared by the method for the present invention can be polished only comprising polyurethanes reaction product
The polishing layer stacked on layer or subpad or sublayer.Polishing pad or stack pad in the case of, the polishing layer of polishing pad of the invention
Suitable for porosity configuration and it is non-porous or be not filled by configuration the two.
Preferably, the average thickness of polishing layer used in the chemical mechanical polishing pads of the present invention arrives for 500 microns
3750 microns (20 mils to 150 mils) or more preferably 750 microns to 3150 microns (30 mils to 125 mils) or more excellent
1000 microns to 3000 microns of selection of land (40 mils to 120 mils) or most preferably 1250 microns to 2500 microns (50 mils arrive
100 mils).
The chemical mechanical polishing pads of the present invention optionally further include at least one additional layer connect with polishing stratum boundary.It is excellent
Selection of land, chemical mechanical polishing pads optionally additionally comprise compressible subpad or are adhered to the base of polishing layer.Compressible base is excellent
Selection of land improves the compliance on the surface of polishing layer and the substrate being polished.
The polishing layer of the chemical mechanical polishing pads of the present invention has the polished surface for being suitable for polishing substrate.Preferably, polish
Surface has at least one huge texture in perforation and slot.Perforation can pass through from polished surface extension or all
The thickness of polishing layer.
Preferably, slot configures on a polished surface so that at least one after rotating chemical mechanical polishing pads during polishing
The surface of the substrate for polishing that slot is inswept.
Preferably, the polishing layer of chemical mechanical polishing pads of the invention has the polished surface for being suitable for polishing substrate, wherein
The polished surface have huge texture, it includes wherein formed and selected from curved groove, linear grooves, perforation with and combinations thereof
Groove pattern.Preferably, groove pattern includes multiple slots.It is highly preferred that groove pattern is designed selected from slot, such as selected from the group being made up of
One kind：Locked groove (can be annular or spiral shape), curved groove, intersecting hachure slot (such as are configured to the X-Y throughout pad surface
Grid), other conventional designs (such as hexagon, triangle), tire tread type pattern, it is irregular design (such as fractal pattern) with
And combinations thereof.It is highly preferred that slot design is selected from the group being made up of：With trough, locked groove, spiral slot, intersecting hachure slot,
X-Y grid grooves, hex shaped groove, vee gutter, divide shape slot with and combinations thereof.Most preferably, it is formed with helicla flute in polished surface
Pattern.Channel profiles are preferably chosen from the rectangle with straight side wall or slot cross-section can be " V " shape, " u "-shaped, sawtooth and its group
It closes.
According to the method for manufacturing polishing pad according to the present invention, chemical mechanical polishing pads can be in its polished surface with huge
Texture or groove pattern molding polish chip to improve slurry flow and be removed from pad-wafer interface.This kind of slot can be from mold
The shape on surface is formed in the polished surface of polishing pad, i.e., wherein mold have huge texture concave surface shape pattern.
The chemical mechanical polishing pads of the present invention can be used for polishing in magnetic substrates, optical substrate and Semiconductor substrate
At least one substrate.
The CMP pad of the present invention is for interlayer dielectric (interlayer dielectric, ILD) and inorganic oxide
Polishing is effective.
Preferably, the method for polishing substrate of the invention includes：It provides selected from magnetic substrates, optical substrate and semiconductor lining
At least one substrate (preferably Semiconductor substrate, such as semiconductor crystal wafer) in bottom；Chemical machinery according to the present invention is provided
Polishing pad；Dynamic Contact is generated between the polished surface and substrate of polishing layer to polish the surface of substrate；And it is adjusted with grinding
It saves agent and adjusts polished surface.
Adjust polishing pad be included in pause polishing when CMP process in intermittent breaks during (" ex situ ") or
During CMP process carries out when (" original position "), adjusting disk is made to be contacted with polished surface.Adjusting disk has usually by by microcosmic groove
Incision pads the coarse adjusting surface of the diamond point composition of the insertion on surface, grinding and ploughing cushion material and updates polishing line
Reason.In general, adjusting disk in the fixed position rotation of rotation axis compared with polishing pad, and cleared away as polishing pad rotates
Annular adjustment region.
Example：
Mixer/aerosol component is the promise letter disposable static mixers of series 160AA, equipped with Nordson Air
CapTMAir blast component, the promise letter EFD. (Nordson EFD, Providence, RI) of Rhode Island Providence).Air
Closure assemblies are commonly referred to as air blast nozzle, are designed to the end of the static mixer of nozzle of the adaptation with given pore size
End.Air blast nozzle only in static mixer nozzle downstream by gas source (such as nitrogen or air) high speed feed-in, with
It is aerosolized to be carried out to it that PU mixtures leave the end of static mixer.Static mixer and air closure assemblies are all one
Secondary property.The composition that CMP pad is prepared for spraying is shown in the following table 1 and 2.Whole amount in table 1 and 2 is by solid
The parts by weight of meter.
Table 1：Two components compositions
1. the English Weida (Invista, Wichita, KS) of Kansas State Wichita；2. the section of philadelphia, pa gathers
Sub- company (Chemtura Corp., Philadelphia, PA)；3. the figure new high-tech material advanced in years of New York Waterford
(Momentive Performance Materials,Waterford,NY)；4. the Dow Chemical of available
(The Dow Chemical Co.,Midland,MI)。
Table 2：Two components compositions
1. the English Weida (Invista, Wichita, KS) of Kansas State Wichita；2. the section of philadelphia, pa gathers
Sub- company (Chemtura Corp., Philadelphia, PA)；3. the figure new high-tech material advanced in years of New York Waterford
(Momentive Performance Materials,Waterford,NY)；4. the Dow Chemical of available
(The Dow Chemical Co.,Midland,MI)；5. Akzo Nobel N.V. (Akzo of Arnhem, netherlands
Nobel,Amsterdam,Netherlands)。
Composition is pumped into static mixer under absolute pressure 110kPa, is mixed in static mixer, and
The 570mm diameter Teflon moulds with concave surface form are applied under ambient pressure, this can generate base thickness
The CMP pad of 3mm, and with the huge line of a succession of annular concentric narrow and long rectangular protrusion form extended from base mat
Reason, the cross sectional dimensions of protrusion is 1.25mm wide and 0.8mm high.Spray flow is controlled by the pump speed into static mixer
Body flow rate.
Example 1：Composition in upper table 1 sprays under 141.6L/min air blast flow rate of gas, at 100 DEG C
Cure 14 it is small when and demould.Resulting articles cross-sectional image analysis shows that average pore size from the top-to-bottom all one of sample
Cause, few air pockets and all be not more than 100 μm.The average pore size in section is 27 μm.Must preferably have and be equal to or small
In 40 μm of aperture.
Example 2A and 2B：Air blast flow rate of gas of the composition in the range of 0-141.6L/min in upper table 2
Lower sprinkling.The following table 3 lists the density of the finished article of the composition using a variety of atomization gas flow rates and being averaged for measurement
Aperture.
Test method：Following test gained molded articles, and the results show is in the following table 2：
Graphical analysis：Gained mechanograph scanning electron micrograph (Scanning electron micrographs,
SEM) deep understanding to aperture average value is provided.Image (not shown) used is the mould specified from the top to bottom in graphical analysis
The section of product (image 1=is pushed up, image 4=bottoms).
DensityIts submergence is compared by the weight of the relatively more given mechanograph of Archimedes method (Archimedes method)
Weight in water measures.
Average pore sizeEach institute is measured by carrying out manual image analysis to selected numerical apertures (250-300 hole)
The aperture of hole is selected, then it is averaged to measure.
Table 3：CMP pad aperture and density
As shown in upper table 3, by the flow rate of gas of air blast lid for realizing small average pore size and required hole
Gap rate is most important.If flow rate of gas is too low, then the fluid spray of generation is appropriate for being formed in shock surface
Excessively thick and/or speed is too low for the bubble of size.Therefore, according to the present invention, the porosity of CMP pad and average pore size can
To change only by the flow rate of gas for changing the air blast lid in equipment.Therefore, in example 2A or even quiet
Very big hole can also be formed when being thoroughly mixed in state mixer；And apply and cured polyurethanes reaction product
Aperture it is unrelated with the amount or quality mixed in static mixer.
On average pore size, upper table 2 is shown as flow rate from 141.6 standard liter/mins (L/min) drops to 56.6L/
Min, the average-size of hole dramatically increase, and number of apertures declines.Based on these data, air flow rate is preferably
85L/min is most preferably 141.6L/min to realize required CMP pad average pore size.The density of mechanograph is flowed with gas
Rate is inversely proportional, the about 0.95gm/cc under the about 0.8gm/cc under highest flow rate of gas to minimum flow rate of gas.Tool
The composition for having trace element provides the density and average pore size in preferred scope of CMP pad.
As shown in upper table 3, method of the invention realizes spray reaction mixture, by retaining environment sky as indicated above
Gas generates hole by adding polymeric microspheres.In example 2, article is sprayed with microsphere, microsphere sets are into major part
The hole observed.This confirms the fabulous control of porosity and predictability.The uniformity instruction of average pore size in overhead line
Microsphere keeps complete in entire technique.The article of example 1 has similar density and only in the case of no polymeric microspheres
The hole generated by embedding air, so as to prove the flexibility of the method for the present invention.
Claims (10)
1. a kind of method for forming chemical-mechanical planarization (CMP) polishing pad, comprising respectively to quiet with nozzle in downstream
Two kinds are introduced in state mixer to arrive under 200kPa absolute pressures without solvent and generally water-free component, each comfortable 100
Liquid polyhydric alkoxide component with temperature T1 and the liquid isocyanate component with temperature T2, the liquid polyhydric alkoxide component bag
Containing one or more polyalcohols, amine hardener；And the liquid isocyanate component includes one or more polyisocyanate
Or isocyanate-terminated carbamate prepolymer；Based on the total solid weight of the reaction mixture, at least one component
Nonionic surfactant comprising the at most sufficient amount of 2.0wt.% is mixed so that hole is promoted to stablize in the static mixer
It closes described two components and forms reaction mixture, under ambient pressure arrange the material flow of the reaction mixture from the nozzle
Go out onto the die substrate with carbamate release surface, and exist in environment temperature to being formed by curing density at 130 DEG C
Porosity polyurethanes reaction product in the range of 0.6gm/cc to 1gm/cc.
2. according to the method described in claim 1, wherein described nozzle is equipped with the atomizing air around the nozzle exterior
Entrance or air blast lid, thus air stream flow through the tip of the nozzle, then along the discharge of the reaction mixture
Material flow flow axially through.
3. according to the method described in claim 1, chemically or physically foaming agent of the wherein described reaction mixture without addition.
4. according to the method described in claim 1, the gelling time of wherein described reaction mixture at curing temperatures is 2 to arrive
300 seconds.
5. according to the method described in claim 1, wherein the liquid polyhydric alkoxide component as the temperature T1 and the temperature T2
When each in liquid isocyanate component is introduced into the static mixer, each there is 1 viscosity for arriving 1000cP.
6. according to the method described in claim 1, wherein in the liquid polyhydric alkoxide component, the amine hardener is aromatic series
Diamines.
7. according to the method described in claim 1, wherein described liquid polyol component additionally comprises various trace elements.
8. according to the method described in claim 1, wherein in the liquid isocyanate component, the isocyanates includes virtue
The carbamate prepolymer of fragrant adoption isocyanates or aromatic isocyanate sealing end.
9. according to the method described in claim 1, wherein described die substrate includes the open type mould with concave surface form
Tool, the configuration of surface fill the required groove pattern of the mold formation CMP pad with the reaction mixture of the application.
10. it is included according to the method described in claim 1, wherein curing the reaction mixture first in environment temperature to 130
Cure the period of 1 to 30 minutes at DEG C, the polyurethanes reaction product is removed from the mold, then finally 60
Porosity article is formed to 1 minute period to 16 when small is cured at a temperature of 130 DEG C.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US15/365,329 US20180147689A1 (en) | 2016-11-30 | 2016-11-30 | Aerosol methods for making chemical mechanical planarization (cmp) polishing pads |
| US15/365329 | 2016-11-30 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108115592A true CN108115592A (en) | 2018-06-05 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711227509.XA Pending CN108115592A (en) | 2016-11-30 | 2017-11-29 | It is used to prepare chemical-mechanical planarization（CMP）The aerosol method of polishing pad |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US20180147689A1 (en) |
| JP (1) | JP2018108634A (en) |
| KR (1) | KR20180062376A (en) |
| CN (1) | CN108115592A (en) |
| TW (1) | TW201825561A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119017280B (en) * | 2024-10-29 | 2024-12-27 | 深圳市鑫德普科技有限公司 | Honeycomb CMP chemical mechanical polishing pad and preparation process thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100471583C (en) * | 2003-06-27 | 2009-03-25 | 雷克蒂塞尔公司 | Method for producing a molded article comprising a sprayed polyurethane layer |
-
2016
- 2016-11-30 US US15/365,329 patent/US20180147689A1/en not_active Abandoned
-
2017
- 2017-11-20 JP JP2017222399A patent/JP2018108634A/en active Pending
- 2017-11-27 KR KR1020170159298A patent/KR20180062376A/en not_active Withdrawn
- 2017-11-28 TW TW106141307A patent/TW201825561A/en unknown
- 2017-11-29 CN CN201711227509.XA patent/CN108115592A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100471583C (en) * | 2003-06-27 | 2009-03-25 | 雷克蒂塞尔公司 | Method for producing a molded article comprising a sprayed polyurethane layer |
Also Published As
| Publication number | Publication date |
|---|---|
| US20180147689A1 (en) | 2018-05-31 |
| JP2018108634A (en) | 2018-07-12 |
| KR20180062376A (en) | 2018-06-08 |
| TW201825561A (en) | 2018-07-16 |
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Application publication date: 20180605 |