CN101068901A - Adjuvant for chemical mechanical polishing slurry - Google Patents

Adjuvant for chemical mechanical polishing slurry Download PDF

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Publication number
CN101068901A
CN101068901A CNA2005800410698A CN200580041069A CN101068901A CN 101068901 A CN101068901 A CN 101068901A CN A2005800410698 A CNA2005800410698 A CN A2005800410698A CN 200580041069 A CN200580041069 A CN 200580041069A CN 101068901 A CN101068901 A CN 101068901A
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polyelectrolyte
auxiliary
ethylenically unsaturated
graft type
unsaturated monomers
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CN101068901B (en
Inventor
李基罗
金种珌
李政熹
洪政填
洪瑛晙
金鲁马
李安娜
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LG Corp
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LG Chemical Co Ltd
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Priority claimed from PCT/KR2005/004592 external-priority patent/WO2006071063A1/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463—Aqueous liquid suspensions
    • 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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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
    • 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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
    • 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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H01L21/321—After treatment
    • H01L21/32115—Planarisation
    • H01L21/3212—Planarisation by chemical mechanical polishing [CMP]

Abstract

Disclosed is an adjuvant for use in simultaneous polishing of a cationically charged material and an anionically charged material, which forms a adsorption layer on the cationically charged material in order to increase the polishing selectivity of the anionically charged material to cationically charged material, wherein the adjuvant comprises a polyelectrolyte salt containing: (a) a graft type polyelectrolyte that has a weight average molecular weight of 1,000-20,000 and comprises a backbone and a side chain; and (b) a basic material. CMP (chemical mechanical polishing) slurry comprising the above adjuvant and abrasive particles is also disclosed.

Description

The auxiliary that is used for chemical mechanical polishing slurry
Technical field
The present invention relates to the auxiliary of a kind of CMP of being used for (chemically machinery polished) slurry, or being used for the auxiliary that positively charged ion charged materials and negatively charged ion charged materials are polished simultaneously, it forms adsorption layer to improve the polishing selectivity of negatively charged ion charged materials to the positively charged ion charged materials on the positively charged ion charged materials.
Background technology
When microelectronic device constantly was endowed higher integrated level, the planarization process that is used to make such microelectronic device became more and more important.As in order to obtain the part effort of high integrated micro device, multiple interconnect technology (multiple interconnection technique) and multilayer laminated technology (multilayer stacking technique) are generally used for semiconductor wafer.But the non-leveling of implementing a kind of back generation in the above-mentioned technology causes a lot of problems.Therefore, in a plurality of steps of microelectronic device manufacturing process, use planarization process, so that the irregular of wafer surface minimizes.
A kind of in the planarization techniques is CMP (chemically machinery polished).In the CMP technological process, wafer surface is pressed with the polishing pad with respect to the surface rotation, and in polishing process known chemical reagent as the CMP slurry is introduced in the polishing pad.Such CMP technology is finished the leveling of wafer surface by the mode of chemistry and physical action.In other words, the CMP technology be by will being pressed on wafer surface with respect to the polishing pad of surface rotation, and simultaneously by providing the chemically reactive slurry to finish the leveling of wafer surface to the wafer surface with pattern.
An embodiment using the CMP technology is STI (shallow-trench isolation).In the STI technology, form shallow relatively groove, such groove is used to form the field region (field region) of the zone of action (activeregion) on separating wafer surface.
As shown in Figure 1, in STI technology, on semiconductor wafer, form liner oxidation silicon (SiO continuously 2) layer 101 and silicon nitride (SiN) layer 102.Then, on SiN layer 102, form the photoresist material pattern.Then, pattern is as sheltering with photoresist by making, and partially-etched SiN layer 102, pad silicon oxide layer 101 and semiconductor wafer 100 are to form a plurality of grooves 103.
In addition, in order to form the field region, method deposition insulating oxide silicon layer 104 by LPCVD (low-pressure chemical vapor deposition), PECVD (plasma reinforced chemical vapour deposition) or HDPCVD (high density plasma CVD) technology, so that layer 104 filling slot 103, and the surperficial tegillum 104 of SiN layer 102 covers.
Subsequently, polishing insulating oxide silicon layer 104 is up to exposing SiN layer 102.In addition, SiN layer 102 places between the two adjacent zone of action, removes pad silicon oxide layer 101 by etching simultaneously.At last, on the surface of semiconductor wafer, form gate (gate) silicon oxide layer 105.
Here, carry out in the process in the CMP technology of removing insulating oxide silicon layer 104, because different chemistry and physical propertiess, insulating oxide silicon layer 104 demonstrates the different rates of removing with SiN layer 102.
The rate of removing of insulating oxide silicon layer and the ratio of the rate of removing of silicon nitride layer are called as the selectivity of CMP slurry.
When the selectivity of CMP slurry reduced, the amount of the SiN layer of removing by slurry increased.Preferably, the SiN layer is not removed.In other words, the insulating oxide silicon layer should be infinity to the selectivity of SiN layer.But the insulating oxide silicon layer of conventional CMP slurry is low to the polishing selectivity of SiN layer, and it is approximately 4: 1.Therefore, in actual CMP technology, the SiN layer is polished to the degree that surpasses acceptable scope.
As a result, in the CMP process,, remove the SiN layer pattern unevenly according to the position in the wafer.Therefore, the thickness of SiN layer changes in entire wafer.Especially at the same time have that this is a serious problem under the situation of semiconductor wafer of high density patterns and sparse pattern.
Because the problems referred to above, final structure with field region has level error (level difference) between zone of action and field region, cause making surplus (margin) reduction and the transistor and the device quality deterioration of the subsequent step of semiconducter device.In brief, the problem of conventional CMP technology is, even remove the SiN layer pattern that can not obtain to have uniform thickness behind the oxide skin by CMP technology.
For addressing the above problem, a lot of effort have been made in the recent period, to develop the paste compound that a kind of rate of removing of controlling the insulating oxide silicon layer is higher than the polishing rate of SiN layer.For example, in U.S. Patent number 5,614,444; Japan publication 1998-106988,1998-154672,1998-270401,2001-37951,2001-35820 and 2001-319900; With such paste compound is disclosed among Korea S publication 2001-108048,2002-0015697,2003-0039999,2004-0057653,2004-0013299 and the 2003-0039999.
Although constantly the CMP paste compound is carried out deep research and development up to now, to improve the selectivity of being represented by the polishing rate of insulation silicon dioxide layer and the ratio of the polishing rate of SiN layer, this paste compound still has very big room for improvement.
Summary of the invention
Technical problem
Therefore, consider that the problems referred to above make the present invention.An object of the present invention is to provide the auxiliary that the structure of a kind of structure that is used for the positively charged ion charged materials and negatively charged ion charged materials is polished simultaneously, it forms adsorption layer to increase the polishing selectivity of negatively charged ion charged materials structure on the structure of positively charged ion charged materials.The present invention's use comprises weight-average molecular weight and is controlled to be 1,000～20, and the polyelectrolyte salt of 000 graft type polyelectrolyte (ionic polymer or macroion) is so that the reunion of abrasive particle minimizes.
Technical scheme
According to a technical scheme of the present invention, a kind of auxiliary that positively charged ion charged materials and negatively charged ion charged materials are polished simultaneously that is used for is provided, it forms adsorption layer to improve the polishing selectivity of negatively charged ion charged materials on the positively charged ion charged materials, this auxiliary comprises polyelectrolyte salt, described polyelectrolyte salt comprises: (a) weight-average molecular weight is 1,000～20,000 and comprise the graft type polyelectrolyte of main chain and side chain; And (b) base material.The CMP that comprises this auxiliary and abrasive particle also is provided slurry.
According to another technical scheme of the present invention, a kind of auxiliary that comprises polyelectrolyte salt of the CMP of being used for slurry is provided, described polyelectrolyte salt comprises: (a) weight-average molecular weight is 1,000～20,000 and comprises the graft type polyelectrolyte of main chain and side chain; And (b) base material.The CMP that comprises this auxiliary and abrasive particle also is provided slurry.
According to another technical scheme of the present invention, provide a kind of STI (shallow-trench isolation) method of using above-mentioned CMP slurry.
According to a technical scheme more of the present invention, a kind of polished method of positively charged ion charged materials that suppresses in polishing process by using polyelectrolyte salt is provided, described polyelectrolyte salt comprises: (a) weight-average molecular weight is 1,000～20,000 and comprise the graft type polyelectrolyte of main chain and side chain; And (b) base material.
Description of drawings
Fig. 1 is the schema of explanation conventional STI (shallow-trench isolation) method.
Fig. 2 is the synoptic diagram of demonstration according to the structure of the graft type polyelectrolyte of preferred implementation of the present invention.
Embodiment
Hereinafter illustrate in greater detail the present invention.
The invention is characterized in that using weight-average molecular weight in polishing process is 1,000～20,000 the charged graft type polyelectrolyte of negatively charged ion, polished with the structure of effective inhibition positively charged ion charged materials, the reunion as the particle of abrasive particle is minimized.
Usually, the surface of silicon nitride is that positively charged ion is charged, and silicon oxide surface is that negatively charged ion is charged.Therefore, for improving the polishing selectivity of silicon oxide to silicon nitride, to be adsorbed in as the negatively charged ion electropolymer of polyelectrolyte on the charged silicon nitride of positively charged ion by electrostatic force, and, therefore make the charged silicon oxide of negatively charged ion easier to be polished to stop the charged silicon nitride of positively charged ion polished.
Among the present invention, if the molecular weight of negatively charged ion electropolymer is too low, then this polymkeric substance sparsely or with the form that approaches adsorption layer is adsorbed on the positively charged ion charged materials structure.Therefore, can not in glossing, the adequately protect structure of positively charged ion charged materials.
For guarantee the protection to the positively charged ion charged materials in glossing, the negatively charged ion electropolymer preferably has high molecular.But if molecular weight is too high, then polymkeric substance partly is adsorbed onto the reunion that causes particle on the abrasive particle by Van der Waals force.In addition, the particle of reuniting like this can bring scratch in CMP technology.
Therefore, the invention is characterized in, for making the electrostatic adhesion maximization of negatively charged ion electropolymer on the structure of positively charged ion charged materials, make simultaneously because the absorption of Van der Waals force minimizes, use the graft type polyelectrolyte that comprises main chain and side chain to replace the linear polymerization ionogen.When relatively at the graft type polyelectrolyte of same molecular weight range and linear polymerization ionogen, the backbone length of graft type polyelectrolyte makes agglomeration minimize less than the electrolytical chain length of linear polymerization.In addition, proportional with side chain lengths, the graft type polymer electrolyte mass-energy with the side chain that is grafted on the main chain forms adsorption layer with density polymer higher on the per unit area on the structure of positively charged ion charged materials, and forms bigger thickness (see figure 2).
In brief, according to the present invention, use the graft type polyelectrolyte to replace the linear polymerization ionogen.Described graft type polyelectrolyte can optionally be adsorbed onto on the structure of positively charged ion charged materials with big thickness, and does not need to increase its molecular weight.Therefore; in glossing; protected the structure that has optionally applied the positively charged ion charged materials of graft type polyelectrolyte by electrostatic force, thereby improved the polishing selectivity of negatively charged ion charged materials (for example silicon oxide) positively charged ion charged materials (for example silicon nitride).
Simultaneously, if use, not only can improve the polishing selectivity of negatively charged ion charged materials, and can improve the not polishing selectivity of charged materials according to auxiliary of the present invention.Therefore, as the equivalent of negatively charged ion charged materials, not charged structure is also included within the scope of the present invention.
As shown in Figure 2, be used for graft type polyelectrolyte of the present invention and comprise main chain 200 and side chain 201.Described graft type polyelectrolyte can form polyelectrolyte salt with base material.Can use the graft type polyelectrolyte of other form except that graft type polyelectrolyte salt within the scope of the invention.
According to the present invention, the weight-average molecular weight of described graft type polyelectrolyte is 1,000～20,000, is preferably 3,000～15,000.If the weight-average molecular weight of described graft type polyelectrolyte is lower than 1,000 or be higher than 20,000, then can not obtain stable paste compound.In addition, if the weight-average molecular weight of polyelectrolyte is higher than 20,000, then abrasive particle can be reunited.In addition, under latter event, polyelectrolyte is adsorbed onto on the structure of negatively charged ion charged materials (for example silicon oxide), also be adsorbed onto on the structure of positively charged ion charged materials (for example silicon nitride), so polyelectrolyte is used as protective layer in glossing.Therefore, the polishing rate of the polishing rate of positively charged ion charged materials structure and negatively charged ion charged materials structure reduces simultaneously, thereby causes polishing selectivity to reduce.
Preferably, it is 500～2,000 length that the side chain on the graft type polyelectrolyte preferably has corresponding to molecular weight, and it is 500～15,000 length that the main chain on the graft type polyelectrolyte has corresponding to molecular weight.If the length of side chain is too short, described polyelectrolyte can not fully be exercised defencive function because cladding thickness is little.On the other hand, if the length of side chain is long, then particle aggregation can take place.In addition, if the length of main chain is too short, cause polyelectrolyte absorption poor.On the other hand, if backbone length is long, abrasive particle then can takes place reunite.
The main chain of polyelectrolyte is the main point that participates in electrostatic adhesion.Therefore, in order to be adsorbed onto the structural purpose of positively charged ion charged materials, main chain preferably comprises a large amount of anionic units.For example, such anionic units comprises functional group as hydroxy-acid group as a part.
Compare with main chain, side chain is less to the influence degree of electrostatic adhesion.Therefore, to need not to be negatively charged ion charged for side chain.But side chain should not be cationic.Side chain mainly plays the purpose of the adsorptive coating of the bigger thickness of formation.
The side chain of described graft type polyelectrolyte preferably comprises by polymerization that contains hydroxyl, carboxyl and/or sulfonic ethylenically unsaturated monomers or co-polymerization deutero-big unit.In addition, the main chain of described graft type polyelectrolyte comprises by the ethylenically unsaturated monomers deutero-unit that contains carboxyl.
Usually, the slurry that is used to polish makes water as dispersion medium.Thereby preferred described graft type polyelectrolyte is water-soluble.Therefore, the big unit that also is preferably formed graft type polyelectrolyte side chain is hydrophilic, and preferably comprises the unit (for example comprising hydroxyl, carboxyl and/or sulfonic ethylenically unsaturated monomers) by the monomer derived of high-hydrophilic.
Described big unit is a short chain polymer, and is formed by big monomer derived, and 8～16 inferior monomer polymerizations of described big monomer form and use functional group dead-end.Because if it is long to comprise the side chain of big unit, agglomeration then takes place, if it is too short to comprise the side chain of big unit, then polyelectrolyte can not be exercised defencive function.
PH according to polyelectrolyte salt of the present invention is 4.5～8.8, is preferably 6.0～7.5.If this pH is less than 4.5 or greater than 8.8, then polishing selectivity can not reach competent level.
For example, described graft type polyelectrolyte can make by the method that comprises following steps: (i) at least a inferior monomer of polymerization forms the big monomer of the side chain of graft type polymkeric substance with acquisition; And the monomer copolymerizable of the main chain of (ii) described big monomer and formation graft type polymkeric substance.
Preparation comprises step according to the preferred implementation of the method for graft type polyelectrolyte of the present invention: (i) comprise the radical polymerization of hydroxyl, carboxyl and/or sulfonic ethylenically unsaturated monomers, form the big monomer of the side chain of graft type polymkeric substance with acquisition; And the ethylenically unsaturated monomers copolymerization that comprises carboxyl of the main chain of (ii) described big monomer and formation graft type polymkeric substance.
Usually, described big monomer obtains by the following method: comprise by using and as the chain-transfer agent of thiohydracrylic acid carboxyl is introduced polymer ends, the ethylenic unsaturated group is introduced the method (Japanese publication number clear 43-11224) of polymer ends to wherein adding glycidyl methacrylate then; By using as 2 of addition-breaking type (addition-cleavage type) chain-transfer agent, 4-phenylbenzene-4-methyl-1-pentene prepares big monomer methods (Japanese publication number flat 7-002954); Or by using metal complex to prepare big monomer methods (Japanese publication number flat 6-23209 peace 7-35411 and U.S. Patent number 4,694,054 and 4,886,861) based on cobalt.But in the present invention, the preferred use at the metal complex based on cobalt that shows excellent specific property aspect control molecular weight distribution and the big monomeric purity of gained prepares big monomer.
Preferably, the ethylenically unsaturated monomers that comprises hydroxyl that is used for step (i) is C1～C12 hydroxyalkyl methacrylate, and its object lesson comprises hydroxyethyl methylacrylate, Rocryl 410, methacrylic acid hydroxy butyl ester etc.In addition, the operable ethylenically unsaturated monomers that comprises carboxyl comprises the carboxylic acid monomer as vinylformic acid, methacrylic acid, methylene-succinic acid or toxilic acid.In addition, operablely comprise sulfonic ethylenically unsaturated monomers and comprise styrene sulfonic acid or naphthene sulfonic acid.
If desired, can comprise hydroxyl and/or sulfonic ethylenically unsaturated monomers and the big monomer of the incompatible preparation of ethylenically unsaturated monomers copolymerization that comprises carboxyl by making.In this case, preferably use methacrylic acid or vinylformic acid.
Preferably will comprise hydroxyl and/or sulfonic ethylenically unsaturated monomers is mixed with the ethylenically unsaturated monomers that comprises carboxyl with 100: 0～70: 30, more preferably 95: 5～85: 15 weight ratio.If use the ethylenically unsaturated monomers that comprises carboxyl with the amount that is higher than 30 weight parts, then the gained paste compound can not provide highly selective and stable fully.
Can use metal complex to come the described ethylenically unsaturated monomers of polymerization as chain-transfer agent based on cobalt.In the presence of radical polymerization initiator, carry out polyreaction by solution polymerization with organic solvent.In addition, can in water, come the described ethylenically unsaturated monomers of polymerization by letex polymerization.Especially preferably use solution polymerization.
The metal complex based on cobalt of effect chain-transfer agent comprises two hydrations two (boron two fluoro-dimethyl glyoximes) cobalt (II) or two hydrations two (boron two fluoro-phenylbenzene glyoximes) cobalt (II).
Based on being used for the big monomeric total amount of preparation, preferably with 5～1, the amount of 000ppm is used the metal complex based on cobalt.If this amount is lower than 5ppm, then the big monomeric molecular weight of gained improves rapidly.If this amount is higher than 1,000ppm then has disadvantageous effect based on the metal complex of cobalt to the quality of final paste compound.
Operable polymerization starter comprises the initiator of organo-peroxide or azo-based.More preferably use as 2,2-azo two-4-methoxyl group-2,4-methyl pentane nitrile, 2,2-azo two-2,4-methyl pentane nitrile, 2,2-azo two-isopropyl cyanide, 2,2-azo two-2-methyl-butyronitrile, 2, and 2-azo two-hexamethylene formonitrile HCN (2,2-azobis-cyclohexanecarbonitrile) or 2,2-azo two-cyanogen pentane (2, the initiator of azo-based 2-azobis-cyanopentane).
Based on being used for the big monomeric total amount of preparation, use described polymerization starter with the amount of 0.1～5 weight part.If this amount is lower than 0.1 weight part, then monomeric transformation efficiency is low.If this amount is higher than 5 weight parts, then the big monomeric purity of gained is low.
Operable organic solvent comprises aromatic compound, fatty compounds, ketone, glycol ether, acetic ester, alcohol etc.The object lesson of organic solvent comprises methyl ethyl ketone, Virahol, propylene glycol monomethyl ether and propyl carbinol.
Then, as mentioned above the big monomer of Huo Deing with as comprise the monomer polymerization of the main chain that can form the graft type polymkeric substance of the ethylenically unsaturated monomers of carboxyl, so that final graft type polyelectrolyte to be provided.
As the ethylenically unsaturated monomers that comprises carboxyl, preferably use methacrylic acid or vinylformic acid.Based on the main chain gross weight,, more preferably use the ethylenically unsaturated monomers that comprises carboxyl with the amount of 70 weight parts with the amount of 65～100 weight parts.If this amount is less than 65 weight parts, then can not obtain enough static avidity, so resulting polymers can not be adsorbed on optionally on the structure of positively charged ion charged materials (for example silicon nitride).Therefore, can not prevent that such structure is polished, cause polishing selectivity to reduce.
If desired, when fashionable with big monomer copolymerization, comprise carboxyl ethylenically unsaturated monomers can with can unite use with the polymerisable monomer that comprises vinyl of its copolymerization.
Although the polymerisable monomer that comprises vinyl is not specifically limited, it is because good reactivity and preferred (methyl) acrylate monomer that uses, and based on the gross weight of main chain, uses such monomer with the amount of 35 weight parts at the most.If this amount is higher than 35 weight parts, then can not finish absorption by static avidity.In addition, as being used as tensio-active agent, the hydrophobic monomer that comprises vinyl has increased the hydrophobicity of main chain, has therefore increased the generation of bubble in final paste compound.
Be used to form the initiator of the main chain of graft type polyelectrolyte, preferably use the organic peroxy initiator.The object lesson of described initiator comprises benzoyl peroxide, lauryl peroxide, t-butylperoxy pivarate, t-amyl peroxy pivalate, uncle's hexyl peroxidation pivalate, tert-butyl hydroperoxide neodecanoic acid ester, uncle's hexyl peroxidation ethylhexoate (t-hexylperoxyethyl hexanoate) etc.
The organic solvent that uses in the main chain of preparation graft type polyelectrolyte comprises and prepares the solvent phase example together that uses in the side chain of same polyelectrolyte.
In addition, by using base material, described graft type polyelectrolyte can be converted into graft type polyelectrolyte salt at aqueous phase.
When auxiliary of the present invention was used for the CMP slurry, spendable base material comprised being selected from and comprises ammonium hydroxide (NH 4OH) with as at least a material of the group of the basic amine of tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide and tetrabutylammonium hydroxide.
Except above-mentioned auxiliary, the present invention also provides a kind of CMP slurry, and it comprises: (i) comprise (a) weight-average molecular weight and be 1,000～20,000 and comprise the graft type polyelectrolyte of main chain and side chain and (b) auxiliary of base material; (ii) abrasive particle; And (iii) water.
Preferably in the CMP slurry, use described polyelectrolyte salt with the amount of 0.1～10wt%.If this amount is lower than 0.1wt%, then polishing selectivity reduces.On the other hand, if this amount is higher than 10wt%, then polishing selectivity reduces, and the reunion of abrasive particle takes place.
Amount with 0.1～10wt% is used described abrasive particle in the CMP slurry.If this amount is lower than 0.1wt%, the height that then can not fully obtain oxide skin is removed rate.Another invention, if this amount is higher than 10wt%, then slurry presents poor stability.
As abrasive particle, can use nano-scale ceramic abrasive grain as silicon-dioxide, aluminum oxide, zirconium white, titanium dioxide and cerium oxide particles.The preferred cerium oxide particles that uses.
Can be by the polyelectrolyte salt that is dissolved in the solvent (for example water), or prepare described CMP slurry by the abrasive particle that is scattered in the dispersion medium (for example water).Preferably, the concentration of the aqueous solution of polyelectrolyte salt is 3～3.5wt%, and the concentration of the aqueous dispersion of abrasive particle is 4～6wt%.
Therefore, the water that forms the CMP slurry can come the water in the composition that comprises polyelectrolyte salt or abrasive particle of being present in of the aqueous solution freely.The amount that is adjusted to 100wt% with the gross weight with slurry makes water.Preferably the amount with 94～99.8wt% makes water.If this amount is lower than 94wt%, then described slurry stability decreases.If this amount is higher than 99.8wt%, the rate of then removing reduces.
In addition, the invention provides a kind of STI (shallow-trench isolation) method of using described CMP slurry.
When using, because silicon oxide layer is to the highly selective of silicon nitride layer, so can remove the SiN layer equably in the CMP technological process in the entire area of wafer according to CMP slurry of the present invention.Therefore, can make the minimize variations of thickness.As a result, the level of zone of action (lcvel) is little with the horizontal difference of field region, can disadvantageous effect not arranged to the quality of transistor and microelectronic device simultaneously.In addition, can use and have high polishing selectivity and the low paste compound of abrasive particle reunion degree advances new CMP technology.Therefore, the present invention is suitable for being applied in the manufacturing of the semiconducter device that needs miniature image (micropattcrn), has therefore formed high-quality miniature image, and has improved reliability and productive rate.
In addition, the invention provides a kind of polyelectrolyte salt that in polishing process, uses and suppress the polished method of positively charged ion charged materials, described polyelectrolyte salt comprises: (a) weight-average molecular weight is 1,000～20,000 and comprises the graft type polyelectrolyte of main chain and side chain and (b) base material.
The charged graft type polymkeric substance of positively charged ion that comprises main chain and side chain by use in polishing process suppresses the polished method of negatively charged ion charged materials and is also included within the scope of the present invention.
In detail with reference to preferred implementation of the present invention.Should be appreciated that following embodiment only is illustrative, the invention is not restricted to this.
Embodiment 1. is used for the preparation of the auxiliary of CMP slurry
(big monomeric preparation)
In the 500mL four-hole boiling flask that has been equipped with agitator, thermometer, nitrogen inlet and condenser, add 75 weight part Virahols, and this mixture bubbled about 20 minutes with nitrogen under reflux temperature.Then, with 0.032g two (boron difluorodiphenyl base glyoxime) cobalt (II) (bis (borondifluorodiphenyl glyoxime) CoII)) be dissolved in the methyl ethyl ketone of 80g, and with about 270 minutes it is dropwise joined in the above-mentioned reactor.Meanwhile, respectively with about 240 minutes and 270 minutes dropwise add the methacrylic acid that comprises 10 weight parts and 90 weight parts hydroxyethyl methylacrylate monomer and be dissolved in the 49g Virahol, comprise 1g2, the polymerization starter solution of 2-azo two-2-methyl-butyronitrile.After adding polymerization starter solution, reaction mixture kept under reflux temperature about 30 minutes, was cooled to room temperature then, was 35% large monomer solution with the acquisition solid content.Use the described big monomer of NMR spectrometer analysis, and big monomeric molecular weight is 1,300, the polymkeric substance degree is 10.Behind this big monomer of thermogravimetry analysis, big monomeric purity is about 92%.
(preparation of graft type polyelectrolyte)
The methacrylic acid of methyl methacrylate, 2.9 parts by weight of acrylic and 4.2 weight parts of the above-mentioned big monomer of the Virahol of adding 120 weight parts, 30 weight parts, 2.9 weight parts in the 500mL four-hole boiling flask that has been equipped with agitator, thermometer, nitrogen inlet and condenser, this mixture bubbled under reflux temperature about 10 minutes
In mixture, add the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester of 0.2 weight part as initiator, and with about 2 hours dropwise adding comprise the monomer of methacrylic acid of methyl methacrylate, 17.2 parts by weight of acrylic and 25.6 weight parts of 17.2 weight parts and the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester of 1.0 weight parts.Then, with 10 minutes dropwise to the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester that wherein adds 0.3 weight part, reaction mixture placed under the reflux temperature about 10 minutes, was cooled to room temperature then, was about 38% graft type polyelectrolyte solution to obtain solid content.After GPC (gel permeation chromatography) assay products, the weight-average molecular weight of this graft type polyelectrolyte is 10,000.The characteristic peak that the NMR analysis of product and thermogravimetric analysis do not show unsaturated carbon atom.
(preparation of graft type polyelectrolyte salt)
In the solution of the graft type polyelectrolyte that makes as mentioned above, add ammonium hydroxide aqueous solution, polyelectrolyte is converted into polyelectrolyte salt, and under vacuum decompression, remove remaining Virahol, the aqueous solution that be 10.5% to obtain solid content, pH is 6.5 graft type polyelectrolyte salt.
(being used for the preparation of the auxiliary of CMP slurry)
In the solution of graft type polyelectrolyte salt, add entry, reach 3wt% up to ultimate density.Adding ammonium hydroxide in the solution of dilution, is 7.1 with the pH that controls solution.At last, obtain to be used for the final auxiliary of CMP slurry.
Embodiment 2 is used for the preparation of the auxiliary of CMP slurry
(big monomeric preparation)
To prepare big monomer with embodiment 1 described same procedure.
(preparation of graft type polyelectrolyte)
Add the Virahol of 120 weight parts, the above-mentioned big monomer of 30 weight parts, the methyl methacrylate and 7.1 parts by weight of acrylic of 2.9 weight parts in the 500mL four-hole boiling flask that has been equipped with agitator, thermometer, nitrogen inlet and condenser, this mixture bubbled under reflux temperature about 10 minutes.
In mixture, add the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester of 0.2 weight part as initiator, and with about 2 hours dropwise adding comprise methyl methacrylate and the monomer of 42.8 parts by weight of acrylic and the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester of 1.0 weight parts of 17.2 weight parts.Then, with 10 minutes dropwise to the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester that wherein adds 0.3 weight part, reaction mixture placed under the reflux temperature about 10 minutes, was cooled to room temperature then, was about 37% graft type polyelectrolyte solution to obtain solid content.After GPC (gel permeation chromatography) assay products, the weight-average molecular weight of this graft type polyelectrolyte is 10,000.The characteristic peak that the NMR analysis of product and thermogravimetric analysis do not show unsaturated carbon atom.
(preparation of graft type polyelectrolyte salt)
To obtain graft type polyelectrolyte salt with embodiment 1 described same procedure.
(being used for the preparation of the auxiliary of CMP slurry)
To obtain to be used for the auxiliary of CMP slurry with the described same procedure of embodiment 1.
Embodiment 3 is used for the preparation of the auxiliary of CMP slurry
(big monomeric preparation)
The methacrylic acid that replaces comprising 10 weight parts except that the hydroxyethyl methylacrylate that uses 100 weight parts and the hydroxyethyl methylacrylate blended monomer of 90 weight parts, with embodiment 1 described same procedure acquisition large monomer solution.The big monomeric molecular weight that obtains among this embodiment is 1,000, and the polymerization degree is 8, and purity is about 96%.
(preparation of graft type polyelectrolyte)
Add the Virahol of 120 weight parts, the above-mentioned big monomer of 30 weight parts, the methyl methacrylate and 5.3 parts by weight of acrylic of 4.3 weight parts in the 500mL four-hole boiling flask that has been equipped with agitator, thermometer, nitrogen inlet and condenser, this mixture bubbled under reflux temperature about 10 minutes.
In mixture, add the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester of 0.2 weight part as initiator, and with about 2 hours dropwise adding comprise the monomer of methacrylic acid of methyl methacrylate, 34.3 parts by weight of acrylic and 25.6 weight parts of 25.7 weight parts and the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester of 1.0 weight parts.Then, with 10 minutes dropwise to the peroxidation PIVALIC ACID CRUDE (25) tert-pentyl ester that wherein adds 0.3 weight part, reaction mixture placed under the reflux temperature about 10 minutes, was cooled to room temperature then, was about 38% graft type polyelectrolyte solution to obtain solid content.
After GPC (gel permeation chromatography) assay products, the weight-average molecular weight of this graft type polyelectrolyte is 10,000.The characteristic peak that the NMR analysis of product and thermogravimetric analysis do not show unsaturated carbon atom.
(preparation of graft type polyelectrolyte salt)
To obtain graft type polyelectrolyte salt with embodiment 1 described same procedure.
(being used for the preparation of the auxiliary of CMP slurry)
To obtain to be used for the auxiliary of CMP slurry with the described same procedure of embodiment 1.
The preparation of embodiment 4.CMP slurry
With volume ratio is to mix the ceria slurry composition as abrasive particle composition (HIHC-1, LG Chemical Ltd.) of 5wt% at 1: 3: 3, prepare the CMP slurry according to auxiliary that is used for the CMP slurry and the water of embodiment 1.
The preparation of embodiment 5.CMP slurry
Except that the auxiliary that be used for CMP slurry of auxiliary replacement that is used for the CMP slurry that uses according to embodiment 2, to prepare the CMP slurry with embodiment 4 described identical methods according to embodiment 1.
The preparation of embodiment 6.CMP slurry
Except that the auxiliary that be used for CMP slurry of auxiliary replacement that is used for the CMP slurry that uses according to embodiment 3, to prepare the CMP slurry with embodiment 4 described identical methods according to embodiment 1.
Use is carried out following test according to each CMP slurry of the foregoing description 4～6, removes rate (/min), nitride layer are removed rate (/min) and polishing selectivity to measure pH, average agglomerated particles size (nm), oxide skin.The results are shown in following table 1.
(a) use pH measuring apparatus (healthy and free from worry pH meter 445) to measure pH.
(b) use light scattering device (dynamic light scattering, Microtrap UPA150, Honeywell Inc., the U.S.) to measure average agglomerated particles size.
(c) use the Nanospec 6100 that buys from Nai Nuo company, before and after polishing, measure the thickness of oxide skin, then calculated thickness difference and obtain oxide skin and remove rate.
(d) use the Nanospec 6100 that buys from Nai Nuo company, before and after polishing, measure the thickness of nitride layer, then calculated thickness difference and obtain nitride layer and remove rate.
(c) record selectivity with the oxide skin rate of removing divided by the nitride layer rate of removing.
[table 1]
Embodiment 4 Embodiment 5 Embodiment 6
The concentration (wt%) that is used for the auxiliary of CMP slurry 1.3 1.3 1.3
pH 7.66 7.35 7.00
Average agglomerated particles size (nm) 535 685 734
Oxide skin is removed rate (/min) 3,134 3,935 3,201
Nitride layer is removed rate (/min) 42 43 43
Selectivity 74.6 91.5 74.4
The preparation of comparative example 1 and embodiment 7～10 CMP slurries
At first, be to mix the ceria slurry composition (abrasive particle composition, HIHC-1, LG Chemical Ltd.) of 5wt% at 1: 7 and with volume ratio according to the auxiliary that is used for the CMP slurry of embodiment 1.Then, water is used for mixture diluted the concentration of auxiliary of CMP slurry to 0wt% (comparative example 1), 0.42wt% (embodiment 7), 0.85wt% (embodiment 8), 1.3wt% (embodiment 9) and 1.5wt% (embodiment 10) with adjustment.
Measuring the pH according to each CMP slurry of comparative example 1 and embodiment 7～10, average agglomerated particles size (nm), oxide skin with method same as described above removes rate (/min), nitride layer is removed rate (/min) and polishing selectivity.The results are shown in following table 2.
[table 2]
The comparative example 1 Embodiment 7 Embodiment 8 Embodiment 9 Embodiment 10
The concentration (wt%) that is used for the auxiliary of CMP slurry 0.0 0.42 0.85 1.3 1.5
pH 7.84 7.93 7.83 7.72 7.67
Average agglomerated particles size (nm) 240 881 835 617 557
Oxide skin is removed rate (/min) 3,854 3,516 3,145 2,944 2,761
Nitride layer is removed rate (/min) 829 66 37 38 40
Selectivity 5 53 85 77 69
The comparative example 2
(being used for the preparation of the auxiliary of CMP slurry)
Remove to use to comprise outside the solution of polyelectrolyte salt that weight-average molecular weight is 10,000 polyacrylic linear anionoid polymerization ionogen and sodium hydroxide, repeat embodiment 1, to be provided for the auxiliary of CMP slurry.
(preparation of CMP slurry)
With volume ratio is to mix the auxiliary that is used for the CMP slurry of the ceria slurry composition as abrasive particle composition (HIHC-1, LG Chemical Ltd.) of 5wt%, above-mentioned acquisition and water at 1: 3: 3 and prepare the CMP slurry.
The comparative example 3
(being used for the preparation of the auxiliary of CMP slurry)
Except using the commercially available glidant that gets (glidant) (trade(brand)name CD-WB, LG Chemical Ltd.), be that weight-average molecular weight is 21,000, and comprise outside the polyelectrolyte salts solution of the anionoid polymerization ionogen represented by structure shown in Figure 2 and sodium hydroxide, repeat embodiment 1, to be provided for the auxiliary of CMP slurry.
(preparation of CMP slurry)
With volume ratio is to mix the auxiliary that is used for the CMP slurry of the ceria slurry composition as abrasive particle composition (HIHC-1, LG Chemical Ltd.) of 5wt%, above-mentioned acquisition and water at 1: 3: 3 and prepare the CMP slurry.
The comparative example 4
(being used for the preparation of the auxiliary of CMP slurry)
Except using commercially available glidant (the trade(brand)name CD-WR that gets, LG Chemical Ltd.), be that weight-average molecular weight is 25,000, and comprise outside the polyelectrolyte salts solution of the anionoid polymerization ionogen represented by structure shown in Figure 2 and sodium hydroxide, repeat embodiment 1, to be provided for the auxiliary of CMP slurry.
(preparation of CMP slurry)
With volume ratio is to mix the auxiliary that is used for the CMP slurry of the ceria slurry composition as abrasive particle composition (HIHC-1, LG Chemical Ltd.) of 5wt%, above-mentioned acquisition and water at 1: 3: 3 and prepare the CMP slurry.
Measuring the pH according to each CMP slurry of comparative example 2～4, average agglomerated particles size (nm), oxide skin with method same as described above removes rate (/min), nitride layer is removed rate (/min) and polishing selectivity.The results are shown in following table 3.
[table 3]
The comparative example 2 The comparative example 3 The comparative example 4
The concentration (wt%) that is used for the auxiliary of CMP slurry 1.3 1.3 1.3
pH 7.29 8.25 7.93
Average agglomerated particles size (nm) 967 806 758
Oxide skin is removed rate (/mm) 2,703 4,092 4,117
Nitride layer is removed rate (/min) 49 903 408
Selectivity 55 4.5 10.1
As above shown in the table 3, use molecular weight to be higher than 20,000 anionoid polymerization ionogen (comparative example 3 and 4) and cause polishing selectivity to reduce.
Therefore, from result shown in last table 1～3 as can be seen, compare with each CMP slurry according to comparative example 1～4, according to CMP slurry of the present invention (embodiment 4～10) demonstrate identical or improved average agglomerated particles size, oxide skin removes rate and nitride layer is removed rate.Especially CMP slurry according to the present invention can provide excellent polishing selectivity.
Industrial applicibility
As mentioned above, be applied to the method that positively charged ion charged materials and negatively charged ion charged materials are polished simultaneously according to the auxiliary of the CMP of being used for slurry of the present invention, it comprises polyelectrolyte salt, and this polyelectrolyte salt comprises weight-average molecular weight and controls to 1,000～20,000 graft type polyelectrolyte.Among the present invention, described polyelectrolyte salt forms adsorption layer on the structure of positively charged ion charged materials, with the polishing selectivity of the structure that increases the negatively charged ion charged materials, and the reunion of abrasive particle is minimized.
Though in conjunction with thinking the most practical at present and preferred embodiment invention has been described, should be appreciated that, the invention is not restricted to disclosed embodiment and accompanying drawing.On the contrary, its plan covers the essence of claims and the numerous modifications and variations in the scope.

Claims (19)

1, a kind ofly is used for the auxiliary that positively charged ion charged materials and negatively charged ion charged materials are polished simultaneously, it forms adsorption layer on the positively charged ion charged materials, to increase the polishing selectivity of negatively charged ion charged materials, wherein said auxiliary comprises polyelectrolyte salt, and this polyelectrolyte salt comprises:
(a) weight-average molecular weight is 1,000～20,000 and comprises the graft type polyelectrolyte of main chain and side chain; And
(b) base material.
2, a kind of auxiliary that is used for CMP (chemically machinery polished) slurry, it comprises polyelectrolyte salt, and this polyelectrolyte salt comprises:
(a) weight-average molecular weight is 1,000～20,000 and comprises the graft type polyelectrolyte of main chain and side chain; And
(b) base material.
3, auxiliary according to claim 1 and 2, wherein, it is 500～2,000 length that described side chain has corresponding to molecular weight, and described main chain to have corresponding to molecular weight be 500～15,000 length.
4, auxiliary according to claim 1 and 2, wherein, described graft type polyelectrolyte comprises:
By comprising at least a ethylenically unsaturated monomers polymerization that is selected from hydroxyl, carboxyl and sulfonic functional group or copolymerization and the deutero-big unit, as side chain; And
By the ethylenically unsaturated monomers deutero-unit that comprises carboxyl, as main chain.
5, auxiliary according to claim 1 and 2, it obtains by the method that comprises the steps:
(i) at least a inferior monomer of polymerization forms the big monomer of the side chain of graft type polymkeric substance with acquisition; And
(ii) make the monomer copolymerizable of the main chain of described big monomer and formation graft type polymkeric substance.
6, auxiliary according to claim 5, wherein, described graft type polyelectrolyte obtains by the method that comprises the steps:
(i) make and comprise at least a ethylenically unsaturated monomers that is selected from the functional group that comprises hydroxyl, carboxyl and sulfonic group and carry out radical polymerization, to obtain big monomer; And
(ii) make described big monomer and the ethylenically unsaturated monomers copolymerization that comprises carboxyl.
7, auxiliary according to claim 6, wherein, the described ethylenically unsaturated monomers that comprises hydroxyl is C1～C12 hydroxyalkyl methacrylate.
8, auxiliary according to claim 4, wherein, described big unit obtains with the copolymerization that comprises the ethylenically unsaturated monomers of carboxyl by comprising at least a ethylenically unsaturated monomers that is selected from the functional group that comprises hydroxyl and sulfonic group.
9, auxiliary according to claim 8, wherein, comprise at least a gross weight that is selected from the ethylenically unsaturated monomers of the functional group that comprises hydroxyl and sulfonic group based on described, use the described ethylenically unsaturated monomers that comprises carboxyl with the amount of 30 weight parts at the most.
10, auxiliary according to claim 4 wherein, is present in the ethylenically unsaturated monomers institute deutero-unit by comprising carboxyl on the described graft type polyelectrolyte main chain and is derived by methacrylic acid or vinylformic acid and obtain.
11, auxiliary according to claim 4, wherein, based on the gross weight of described main chain, with the amount of 65～100 weight parts use described be present on the graft type polyelectrolyte main chain by the ethylenically unsaturated monomers deutero-unit that comprises carboxyl.
12, auxiliary according to claim 6, wherein, described ethylenically unsaturated monomers that comprises carboxyl and the polymerisable monomer that comprises vinyl are united use in step in (ii).
13, auxiliary according to claim 12, wherein, the described polymerisable monomer that comprises vinyl is (methyl) acrylate monomer.
14, auxiliary according to claim 1 and 2, wherein, described base material (b) is ammonium hydroxide or basic amine.
15, auxiliary according to claim 1 and 2, wherein, the pH of described polyelectrolyte salt is 4.5～8.8.
16, a kind of CMP (chemically machinery polished) slurry, it comprises:
(a) as each described auxiliary in the claim 1～15;
(b) abrasive particle; And
(c) water.
17, CMP slurry according to claim 16, based on the gross weight of the described slurry of 100wt%, it comprises the described auxiliary of 0.1～10wt%, the described abrasive particle of 0.1～10wt% and the water of surplus.
18, a kind of STI (shallow-trench isolation) method of using CMP slurry as claimed in claim 16.
19, a kind of polished method of positively charged ion charged materials that in polishing process, suppresses, it uses polyelectrolyte salt, and this polyelectrolyte salt comprises (a) weight-average molecular weight to be 1,000～20,000 and to comprise the graft type polyelectrolyte of main chain and side chain; And (b) base material.
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KR100786949B1 (en) * 2005-12-08 2007-12-17 주식회사 엘지화학 Adjuvant capable of controlling a polishing selectivity and chemical mechanical polishing slurry comprising the same
KR100832993B1 (en) 2006-04-14 2008-05-27 주식회사 엘지화학 Adjuvant for chemical mechanical polishing slurry
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CN112872916A (en) * 2020-12-28 2021-06-01 深圳市裕展精密科技有限公司 Polishing system and polishing method

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