CN101220255B - Chemical mechanical grinding fluid and chemical mechanical planarization method - Google Patents
Chemical mechanical grinding fluid and chemical mechanical planarization method Download PDFInfo
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Abstract
The invention relates to a chemical and mechanical lapping slurry, in particular to a chemical and mechanical lapping slurry which is capable of removing copper on a piece of design wafer, including an acid, a surfactant, a water-based medium, and a plurality of silicon dioxide lapping particles containing potassium, wherein the surfaces of the particles are modified by a surface electrical property modifier; by means of the structure of the lapped particles, compared with lapping slurry adopted by general industry, the lapping slurry has the advantages that damages of a tantalum nitride barrier to the lapped design wafer can be further avoided; copper covered on the barrier can be stripped more thoroughly; sunken degree formed on the lapped surface of the wafer is less; the whole efficacy is excellent and in accordance with requirements of the industry; besides, a chemical and mechanical flattening method is provided, namely, leading a piece of wafer to be contacted with a polishing pad, conveying the chemical and mechanical lapping slurry containing a plurality of the silicon dioxide lapping particles to the wafer and the polishing pad, and flattening at least partial surface of the wafer.
Description
Technical field
The present invention relates to a kind of grinding milk, particularly relate to and a kind ofly contain several and carry out surfaction, and wrap the chemical and mechanical grinding fluid of potassic silicon-dioxide polishing particles through a kind of surface electrical behavior modification agent.
Background technology
The chemical-mechanical planarization technology has been a ring indispensable in the manufacture of semiconductor, its processing procedure ability not only has direct influence with back segment micro-photographing process result's quality, and along with diameter wafer increases, the processing procedure live width is dwindled, and the variation tendency of the raising of element integration or the like manufacture of semiconductor parameter, compared to the past, industry has stricter requirement for the smooth degree of crystal column surface.Utilize cmp (chemicalmechanical polishing, abbreviate " CMP " as) processing procedure, can make crystal column surface be comprehensive planarization, and the wafer that the advantage of CMP is to break through the IC with densification is in the gold-tinted micro-photographing process, the problem that shoals because of the exposure depth of focus that miniaturization causes; Therefore CMP not only can promote yield, and to the development toward finer ultimate exposure, is very helpful.
Chemomechanical copper grinding (Cu CMP) is of metallochemistry mechanical mill (metalCMP), and it can adopt two stage lapping mode to carry out, to reach better wafer planarization effect; The so-called fs is earlier the metallic copper on surface to be removed, with the barrier layer (its material is generally tantalum nitride (TaN) or metal tantalum (Ta)) under exposing; Subordinate phase then is again that this barrier layer is worn.
This two stage is to use specific grinding milk respectively.Consideration based on the subsequent product yield, in this fs, industry for the requirement of employed grinding milk is, it is smooth more good more to grind the crystal column surface of finishing with this grinding milk, that is to say that its depression (dishing) is light more good more with the degree of abrasion (erosion), and this grinding milk to have height for copper and removes effect, and the crystal column surface that will avoid being ground produces tantalum nitride barrier layer infringement (TaN damage), the worn barrier layer of just trying not.
Cu CMP grinding milk (slurry) is that the polishing particles by liquid state slurry and solid-state shape is constituted, and this slurry then is except water, also includes chemical such as acid, alkali and interfacial agent.With regard to employed grinding milk of above-mentioned fs, chemical in its slurry is dominated the chemical milling effect, that is to say, utilizes its potential of hydrogen that an environment is provided, so that after the metallic copper oxidation of crystal column surface, formation one can be considered the cupric oxide passive film of " but wearing course "; So this grinding milk can be acid or alkaline.Polishing particles then key machine grinds effect, that is to say, by particle itself and this burning passive film mechanical force of mutual friction mutually, this film is removed, and the pattern of wafer is presented.
With regard to the polishing particles aspect, generally speaking its material can be silicon oxide, aluminum oxide, zirconium white, cerium oxide, silicon carbide, titanium oxide, silicon nitride, or these a combination.
So in Cu CMP, be noted that, but the formation of wearing course with remove, need reach balance, otherwise probably cause depression or abrasive phenomenon, make crystal column surface planarization deficiency, it is very huge so will to influence the subsequent product yield; On the other hand, can bring into play its function for making polishing particles, prerequisite is that polishing particles needs stably to disperse to be present in the slurry, can possess the worn ability of falling this wearing course.
Therefore, " grinding milk " is partly to improve at polishing particles or slurry etc. two; For example TW I235761 carries out towards the direction that improves slurry.To be that request is a kind of grind the slurry that grinds that copper base metal uses to this case, comprises silicon-dioxide abrasive substance, oxygenant, Amino acid, three azole compounds, and water; The content of Amino acid and three azole compounds is 5 to 8 than (weight ratios of Amino acid/three azole compounds), and this three azole compounds is by 1,2,3-triazoles, 1,2, chooses in 4-triazole and their group that derivative constituted; And its employed silicon-dioxide abrasive substance promptly is general silicon-dioxide polishing particles.
Often to be used for colloid silica (colloidalsilica) particle, be to prepare with wet chemical (wet chemical method) as polishing particles; Its modus operandi roughly is the first slightly rare water glass of allotment one concentration (sodium silicate (sodium water glass for example, its principal constituent is water glass (sodium silicate), potash water glass (potassium water glass, principal constituent is potassium silicate (potassiumsilicate)) aqueous solution, then this aqueous solution is removed in this aqueous solution for example Na by Zeo-karb
+, K
+Deng alkalimetal ion, and form an active silicic acid (the active silicic acid) aqueous solution, for example add again sodium hydroxide (sodiumhydroxide, NaOH), potassium hydroxide (potassium hydroxide, KOH), ammonium hydroxide (ammonium hydroxide, NH
4OH), or sodium silicate solution cooperates suitable temperature and potential of hydrogen to impose one alkalinisation treatment (alkalization), makes active silicic acid produce the condensation polymerization reaction, and then nucleation grows into solid particulate, and it is colloid silica; The concentrated program that undergoes ultrafiltration again afterwards, and obtain a kind of silicon dioxide gel.Known to the applicant, general industry (can produce stink and human body skin and respiratory tract are had negative impact as ammonium hydroxide based on its operational security and convenience, so often avoid using), considerations such as cost of material and production line planning, mostly above-mentioned alkalinisation treatment is that being made into the aqueous solution with NaOH or sodium silicate carries out.
The surface of this colloid silica particle is electronegative, only can stable existence in the slurry of alkalescence, be unfavorable for that the acid grinding milk of copper chemical grinding fs is used; Fortunately industry is known that after silicon dioxide granule being aided with the processing of surface electrical behavior upgrading, can make its surface by the positively charged ion upgrading (related description that this surface electrical behavior upgrading is handled, can referring to " The Chemistry of Silica-R.K.Iler-WileyInterscience (1979); p.410-441 "), for example when preparing colloid silica with wet chemical, pass through aluminium, chromium, gallium, titanium, and the above metal oxide of the trivalent of zirconium (sodium aluminate (sodium aluminate) for example, chlorination oxyaluminum (aluminium hydroxychl oride)) as the surface electrical behavior modification agent, can make the silica sphere structure by this type of metallic cation absorption bonding, this silica particle surface is electrically changed, therefore particle can stably be present in the tart environment, thereby significantly expanded using value and the scope of colloid silica particle in grinding milk, and can be used as chemomechanical copper grinding polishing particles in the employed acid grinding milk in the fs.
That US 5368833 is asked is a kind of silicon dioxide gel (silica sol), and it has scope is 8～45% S value (S-value), and includes and have 750～1000m
22～25% aluminium atom is arranged in the specific surface area of/g and its particle structure.This case is addressed this silicon dioxide gel in summary be the additive that is particularly suitable for being used as when making paper or other analogous products, and also address this case for second section on specification sheets the 2nd hurdle and be suitable for making the silicon dioxide granule with wider distribution of sizes.
In this case in the literary composition, the mode of this silicon dioxide gel of preparation of being demonstrated, then similar with previous described wet chemical, mainly be after buck glass (being preferably sodium silicate) is made into the aqueous solution, via acidification and alkalinisation treatment so that silicon dioxide granule form, carry out the surfaction program of cationic exchange program and particle more in regular turn, and obtain desirable silicon dioxide gel.With regard to this case specification sheets the 3rd hurdle 9-15 capable described in, alkalinisation treatment in the preparation flow, be to adopt sodium hydroxide, potassium hydroxide, ammonium hydroxide, and water glass alkaline matters such as (as sodium silicate, potash water glasss), and think to be preferably and select water glass for use, particularly collocation has the sodium silicate of the sodium oxide of specified proportion scope, does not so address reason, and does not also have extra description for other alkaline agent.
Because the needed polishing particles of CMP grinding milk, its particle size homogeneity is high more then good more, therefore for those skilled in the art, emphasize to obtain the US 5368833 of " having the silicon dioxide granule of wider distribution of sizes ", the technology that it disclosed also is unfavorable for being made for the polishing particles of CMP grinding milk; On the other hand, this case is explicit word or hint this silicon dioxide gel after adding other material not also, can form a kind of suitable with as in the copper chemical grinding fs, employed acid grinding milk.
What US 6362108 was asked is a kind of grinding composite, it is characterized in that being to include a kind of acidic suspension through the colloid silica of positively charged ion upgrading, this colloid silica particle is to be indivedual shapes (individualized), and with the medium of water as this suspension.This grinding composite is to be applicable to the insulation material layer based on polymer that has a low-k (dielectric constant) to, carries out cmp; But this case does not mention this grinding composite carries out cmp to the layer body (for example metallic copper) of other kind material possibility.
TW I245789 case (filed an application in the U.S. June 14 calendar year 2001 by accomplice, its case number is 09/882,548, publication number is 20030094593) two kinds of slurries of request, a kind of is to comprise a silicon oxide with main particulate aggregate, the size of this aggregate is less than 5 microns, and this silicon oxide has and equals on the surface-area of every square nanometers or more than 7 hydroxy content; Another kind of then be one to be used for removing copper, tantalum, and the slurries of silicon-dioxide from microelectronic substrates, and these slurries comprise a kind of silicon oxide, it includes little equal or more than the content of 7 hydroxys on the surface-area of every square nanometers.
This case has addresses its substrate surface material in order to remove, and comprises silicon, aluminium, silicon oxide, tungsten, titanium, titanium nitride, copper, tantalum, tantalum nitride; The right result who complies with the comparative example 10,11,12 of this case, these slurries remove speed nearly all greater than copper for tantalum, and also ask the efficacy characteristics of described slurries " tantalum is at least 1 with respect to the ratio that removes speed of copper " in the 9th, 25 of its claims, described as can be known slurries mainly are in order to remove tantalum.Because " tantalum " is in order to as one of material of the barrier layer of metallic copper, therefore TW I245789 case two slurries of being asked as can be known, and be not suitable for requiring worn metallic copper and avoiding fs of worn barrier layer of chemomechanical copper grinding, but be applicable to the subordinate phase of the worn barrier layer of chemomechanical copper grinding.
Therefore, just take the two stage manufacturers that carry out chemomechanical copper grinding, for the fs of its grinding, still need one more can grind away the copper layer on the wafer and more can avoid grinding the grinding milk of this barrier layer, so that the copper layer is tried one's best worn after, still can keep the barrier layer under it; On the other hand, the quality of grinding milk and effect about again the yield of follow-up semiconductor product, and the consumption of grinding milk is also very huge in the CMP process, therefore semiconductor manufacturer has acceptable cost, can more grind away the copper layer and avoids grinding away barrier layer for one, and can effectively reduce the grinding milk of the surperficial sinking degree of polished wafer, very urgent demand is arranged.
Summary of the invention
In foregoing wet chemical in order to preparation colloid silica particle, what widely assert is, silicate aqueous solution through the lixiviating metal ion is added highly basic to carry out " alkalinisation treatment " of condensation polymerization reaction, is the critical period that the colloid silica particle forms; Yet just known to the applicant, mostly pertinent literature or patent case are to focus on the operational alkali of explanation to the viewpoint of this " alkalinisation treatment " which, therefore, employed alkali roughly is to reach " convenience of production line pipeline configuration " with " cost is lower ", " tool processing safety " to consider during general the preparation, the most normal use promptly is the NaOH aqueous solution, or also as the sodium silicate aqueous solution of starting raw material; But the colloid silica particle can be denied the difference that shows on the grinding operation of reality on the effect because of using different alkali in the alkalinisation treatment, making, is still still unfathomed mystery in this industry.
As described above, " alkalinisation treatment " is the critical period that the colloid silica particle forms, therefore the applicant thinks the alkali that added this moment, the rerum natura of formed colloid silica particle after should having influence on, also may have influence on the mill capacity of described particle and follow-up prepared grinding milk further, thereby via attempting the back discovery in many ways, if replace the general NaOH aqueous solution that uses with the KOH aqueous solution, impose alkalinisation treatment and carry out the condensation polymerization reaction, then for example using sodium aluminate to be used as a kind of surface electrical behavior modification agent comes the colloid silica particle that is obtained is carried out surfaction, other program is still according to a grinding milk that general fashion obtained, it demonstrates the grinding milk that carries out the condensation polymerization reaction and then obtain with the NaOH aqueous solution than generally unexpectedly when grinding, more can grind away the copper layer of crystal column surface and more can avoid barrier layer to be ground!
Because the period that alkalinisation treatment also forms for the colloid silica particle, with reference to Fig. 1 with and affiliated books in associated viscera, the applicant infers, change with the KOH aqueous solution and carry out the colloid silica particle that alkalinisation treatment was obtained, its structure should be similar with the particle structure shown in Fig. 1, the part of Na will be got by K and be replaced, and-part of " H " on the OH group, then may be replaced by K and form-the OK group; The part of " K " may be dissociateed then, so " OK " group becomes " O-" that has electric charge.But carry out alkalinisation treatment with the KOH aqueous solution, the colloid silica particle that obtains causing is based on which kind of voltinism or rerum natura, and help at follow-up the corresponding grinding milk that obtains, in the fs of chemomechanical copper grinding, also can avoid tantalum nitride to be ground but can more grind away the copper layer, the applicant still fails to know so far.
The objective of the invention is is providing a kind of chemical and mechanical grinding fluid that can more grind away the copper layer of a slice pattern wafer and can avoid grinding away tantalum nitride.
Chemical and mechanical grinding fluid of the present invention comprises: a kind of acid, a kind of interfacial agent, and a kind of aqueous medium; This chemical and mechanical grinding fluid also comprises several and carries out surfaction through a kind of surface electrical behavior modification agent, and potassic silicon-dioxide polishing particles.
In addition, the present invention also provides a kind of chemical mechanical planarization method, comprises the following step: a wafer is contacted with a grinding pad; (B) carry one to have the chemical and mechanical grinding fluid of several silicon-dioxide polishing particles to this wafer and grinding pad; And (C) with this chemical and mechanical grinding fluid with the surface of this wafer to the small part planarization; Described silicon-dioxide polishing particles is to carry out surfaction through a kind of surface electrical behavior modification agent, and contains potassium.
Via the follow-up susceptible of proof of respectively testing, use chemical and mechanical grinding fluid of the present invention and chemical mechanical planarization method, in the fs of chemomechanical copper grinding, really more by the chemical and mechanical grinding fluid of business-like including " with NaOH aqueous solution alkalization and through the colloid silica particle of aluminate surfaction ", and utilization comprises the grinding milk of this kind silicon-dioxide polishing particles and the chemical mechanical planarization method that carries out, more can grind away the copper layer, and more avoid grinding away barrier layer.
Therefore, chemical and mechanical grinding fluid of the present invention under the prerequisite that keeps tantalum nitride, more completely grinds away the copper layer when can more making in the copper wafer fs polish process, and helps next stage to grind the lifting of benefit and the enhancement of subsequent product yield.
Chemical and mechanical grinding fluid of the present invention and chemical mechanical planarization method have the business potential of high degree; Its distributing style is simple, each composition also obtains easily, need not cooperate other specific installation to use, and its embodiment again with habitual roughly identical of present industry, and meet its operating habit, more can grind away the copper layer of wafer again and avoid the infringement of tantalum nitride barrier layer to produce, this type of advantage all very helps semiconductor manufacturer, to create better productivity effect and commercial profit.
Description of drawings
Fig. 1 is a structural representation, be illustrated in the colloid silicon dioxide granule, sodium and other atoms are in locational relativeness, take passages in the Figure 12 of the 24th page of books " THE COLLOIDCHEMISTRY OF SILICA-Developed from a symposiumsponsored by the Division of Colloid and Surface Chemistry; at200th National Meeting of the American Chemistry Society; Washington; DC; August 26-31,1990 ";
Fig. 2 is OM figure, illustrates that the profile of each member has been black via the pattern crystal column surface place behind the cmp, shows herein to cause the infringement of tantalum nitride barrier layer because of grinding;
Fig. 3 is another OM figure, illustrates that the profile of each member is not black via the pattern crystal column surface place behind the cmp, shows herein not cause the infringement of tantalum nitride barrier layer because of grinding.
Embodiment
Chemical and mechanical grinding fluid of the present invention comprises: a kind of acid, a kind of interfacial agent, and a kind of aqueous medium; This chemical and mechanical grinding fluid also comprises several and carries out surfaction through a kind of surface electrical behavior modification agent, and potassic silicon-dioxide polishing particles.
This silicon-dioxide polishing particles is to make by the preparation method that any industry can be thought to reach, after for example an aqueous silicate solution being carried out one decationizing processing, impose alkalinisation treatment with the alkaline matter (for example potassium hydroxide or potash water glass) that contains potassium, carry out particle nucleation growth reaction and form particle, then after coming particle carried out surfaction with a kind of surface electrical behavior modification agent, impose one decationizing by the Zeo-karb tubing string again and handle and obtain.In each concrete example of the present invention, be after carrying out alkalinisation treatment with potassium hydroxide aqueous solution, the colloidal sol that obtained by behind the cationic exchange tubing string, is obtained the desirable silicon-dioxide polishing particles of the present invention and this aqueous medium; After adding acid and interfacial agent successively again, form chemical and mechanical grinding fluid of the present invention.
The program of carrying out of this surfaction is also known by this industry; Preferably, this surface electrical behavior modification agent is aluminium, chromium, gallium, titanium, or the above metal oxide of the trivalent of zirconium, or these a combination; It more preferably is aluminate; More preferably be again sodium aluminate or potassium aluminate.In each concrete example of the present invention, this surface electrical behavior modification agent is a sodium aluminate; And water glass, and the potassium hydroxide and the aluminate that is used for carrying out the surfaction processing that are used for carrying out alkalinisation treatment afterwards, then be to be made into an aqueous solution respectively to use.According to the analytical data that is obtained, calculate with the weight sum total of described silicon dioxide granule in addition, the content of potassium is to account for more than the 100ppm; And just the present invention is to account for more than the 200ppm preferably.
And the production method in the concrete example of chemical and mechanical grinding fluid of the present invention, then being at normal temperatures should acid, interfacial agent, is mixed with this silicon dioxide gel.
As previously mentioned, this industry is known carries out surfaction (in this industry through a kind of surface electrical behavior modification agent, if come polishing particles is carried out surfaction as the surface electrical behavior modification agent with aluminate, then generally claim that described polishing particles is " through the aluminium surfaction " (the particles were modified by aluminum)) the silicon-dioxide polishing particles, be to be fit to be present in the tart environment.Preferably, the pH value of chemical and mechanical grinding fluid of the present invention is between 2～5; More preferably, be between 3～4, just demonstrate as each concrete example among the present invention.
The present invention is for above these particle diameters through the silicon-dioxide polishing particles of aluminium surfaction of carrying, and unrestrictedly, particularly the particle diameter of these particles will change along with the variation of manufacturing conditions.And each concrete example is demonstrated in the present invention, and these particle diameters through the silicon-dioxide polishing particles of aluminium surfaction are between 10～50nm.
In addition the quantity of " the potassic silicon-dioxide polishing particles " that contains in the chemical and mechanical grinding fluid of the present invention is to surpass one, therefore represents with " most " or " several ".The silicon-dioxide polishing particles quantity that contains in the chemical and mechanical grinding fluid particularly of the present invention, be can be by the number of slurries amount, and the various related preparation conditioned disjunction programs of this grinding milk change, so the polishing particles quantity that contains in the chemical and mechanical grinding fluid of the present invention should not have the upper limit.
Acid in the chemical and mechanical grinding fluid of the present invention mainly is residual to suppress it in order to the copper layer on the corrosion copper wafer, or quickens the corrosion of copper layer.In the present invention, preferably, employed acid is propanedioic acid, Succinic Acid, pentanedioic acid, hexanodioic acid, the methyne Succinic Acid, FUMARIC ACID TECH GRADE, vinylformic acid, the 2-oxyacetic acid, formic acid, acetate, caproic acid, lactic acid, oxysuccinic acid, tartrate, glyconic acid, citric acid, hydrochloric acid, sulfuric acid, maleic acid, FUMARIC ACID TECH GRADE, 2, the 2-dimethyl succinic acid, 2-ethyl-2-pyrovinic acid, 2, the 3-dimethyl succinic acid, the methyne Succinic Acid, 2-methyl-maleic acid, 2-methyl-FUMARIC ACID TECH GRADE, 2-methyl-2-oxyacetic acid, 2-ethyl-2-oxyacetic acid, 2,2-diethyl-2-oxyacetic acid, 2-ethyl-2-methyl-2-oxyacetic acid, the 2-methacrylic acid, the 2-ethylacrylic acid, the 3-methacrylic acid, 2, the 3-dimethacrylate, 1,2,3,4-BTCA (1,2,3,4-butanetetracarboxylic acid), or these one the combination.More preferably, selected acid is Succinic Acid, pentanedioic acid, hexanodioic acid, methyne Succinic Acid, FUMARIC ACID TECH GRADE, vinylformic acid, 2-oxyacetic acid, formic acid, 1,2,3,4 BTCA, or these a combination.
Based on this industry and applicant institute cumulative practical experience, the content of employed acid is preferably the 0.01～5wt% that accounts for chemical and mechanical grinding fluid of the present invention; In each concrete example of the present invention, be to use hexanodioic acid separately, or use hexanodioic acid, methyne Succinic Acid, formic acid, 1,2,3, a combination of 4-BTCA, and in each concrete example, the total content scope of acid is 0.4～0.8wt% of pairing chemical and mechanical grinding fluid.
In the present invention, preferably, this interfacial agent is anionic interfacial agent or non-ionic interfacial agent; Based on this industry and China invites the person institute cumulative practical experience, the content of employed interfacial agent is preferably the 0.01～1wt% that accounts for chemical and mechanical grinding fluid of the present invention in addition.And in each concrete example of the present invention, this interfacial agent is an anionic interfacial agent.
For promoting grinding effect or its working life, chemical and mechanical grinding fluid of the present invention, except above-mentioned acid, interfacial agent, aqueous medium, beyond the silicon-dioxide polishing particles, more can comprise the additive that other has its specific function, for example fungistat (can avoid the long bacterium of grinding milk, cause its quality instability or usefulness to change), corrosion inhibitor (can avoid on the copper wafer copper wire by the sour excessive corrosion in the grinding milk), oxygenant (in order to impel the oxidation of copper layer), stablizer various additives such as (in order to stablize the physico-chemical property of grinding milk); Described additive is can separately or mix ground to use.
Preferably, chemical and mechanical grinding fluid of the present invention also comprises a corrosion inhibitor; More preferably, this corrosion inhibitor is to be selected from the group that is made of following: benzotriazole, tricyanic acid, 1,2,3-triazoles, 3-amido-1,2,4-triazole, 3-nitro-1,2,4-triazole, 4-amido-3-diazanyl-1,2,4-triazolyl-5-mercaptan (4-amino-3-hydrazino-1,2,4-triazol-5-thiol) (Popeye gets
), benzotriazole-5-carboxylic acid, 3-amido-1,2,4-triazole-5-carboxylic acid, I-hydroxybenzotriazole, nitrobenzene and triazolam, and these a combination.In each concrete example of the present invention, employed corrosion inhibitor is a benzotriazole.
Preferably, chemical and mechanical grinding fluid of the present invention also comprises an oxygenant; More preferably, this oxygenant is to be selected from the group that is made of following: hydrogen peroxide, iron nitrate, Potassium Iodate, peracetic acid, potassium permanganate, and these a combination.In each concrete example of the present invention, employed oxygenant is a hydrogen peroxide.
With regard to applicant's practical experience, industry can be by the various grinding results or the phenomenon of wafer, and judging whether needs employed chemical and mechanical grinding fluid is additionally added materials.For example, the grinding rate when wafer is lower than 3000
The time, can in chemical and mechanical grinding fluid, increase the content of acid compounds and polishing particles, to promote grinding rate; When the marginal trough degree of the wafer that is ground is too high, then can reduce by increasing the interfacial activity agent content; And when crystal column surface has metal residual, then can lower the metal residual situation by increasing this metal residual inhibitor content.In addition, if the marginal trough degree that desire increases grinding rate and more effectively reduces this crystal column surface also can add formic acid and methyne Succinic Acid in chemical and mechanical grinding fluid.Chemical and mechanical grinding fluid of the present invention also is suitable for above practice operation skill, and as shown in each concrete example model.
Other what deserves to be mentioned is, relevant for the operational details of above-mentioned decationizing processing; The consumption of material such as silicate, potassium hydroxide or the concentration that is suitable for when being made into the aqueous solution etc. become because of; The kind of surface electrical behavior modification agent, acid, interfacial agent and other various additive and the control of content thereof, and potassium content accounts for the ratio of the weight sum total of silicon dioxide granule; The pH value of slurries; The service temperature of each step ... or the like, all be and to cooperate its professional attainment to consider and changed, to obtain a pair of his preferable result according to those skilled in the art's demand.Therefore chemical and mechanical grinding fluid of the present invention, should not be subjected to above-mentioned every change because of restriction.
The present invention also provides a kind of chemical mechanical planarization method, comprises the following step: a wafer is contacted with a grinding pad; (B) carry one to have the chemical and mechanical grinding fluid of several silicon-dioxide polishing particles to this wafer and grinding pad; And (C) with this chemical and mechanical grinding fluid with the surface of this wafer to the small part planarization; And this chemical mechanical planarization method is characterised in that:
Described silicon-dioxide polishing particles is to carry out surfaction through a kind of surface electrical behavior modification agent, and contains potassium.
Same with chemical and mechanical grinding fluid of the present invention, because chemical mechanical planarization method of the present invention, principal character be with described contain potassium and the surface ground a wafer by the silicon-dioxide polishing particles of upgrading, therefore, even if change various wafer, grinding pad, or conversion chemical and mechanical grinding fluid other composition except this silicon-dioxide polishing particles, chemical mechanical planarization method of the present invention all can be implemented.
Embodiment
The present invention will be described further with regard to following examples and comparative example, but will be appreciated that, described embodiment only illustrates, and should not be interpreted as restriction of the invention process.
In addition, if there is not special explanation, the preparation of embodiment and comparative example and follow-up every test and evaluation all are to carry out under the environment of normal temperature and pressure.
[chemical]
The embodiment and the comparative example of following chemical and mechanical grinding fluid of the present invention and chemical mechanical planarization method are to select for use following chemical or equipment to be prepared respectively:
(1) deionized water.
(2) water glass: made by Taiwan Rong Xiang company, model is No. 3.
(3) potassium hydroxide: made by U.S. ACROS company, model is 232550010.
(4) sodium hydroxide: made by U.S. ACROS company, model is 134070010.
(5) sodium aluminate: made by U.S. ACROS company, model is S/2200/60.
(6) cationic exchange tubing string: by applicant's self-control, that place in the tubing string is Rohm﹠amp; Haas company makes, and model is the Zeo-karb of Amberjet 1500H.
(7) hexanodioic acid: by the manufacturing of U.S. TEDIA company.
(8) formic acid: by the manufacturing of U.S. Aldrich company.
(9) methyne Succinic Acid: by the manufacturing of U.S. Aldrich company.
(10) 1,2,3,4-BTCA: by the manufacturing of U.S. Aldrich company.
(11) anionic interfacial agent.
(12) hydrogen peroxide: by Taiwan Bo Lv limited-liability company (TAIWANMAXWAVE CO., LTD.) manufacturing.
The preparation of [embodiment 1-4] chemical and mechanical grinding fluid
The sodium silicate of 300ml is mixed back formation one sodium silicate aqueous solution with the deionized water of 2700ml, with it by behind the Zeo-karb tubing string, under 80 ℃ (in practice operation last 70～80 ℃ all can), adding a concentration by amount is the KOH aqueous solution of 5wt%,, react greater than 10 up to the pH of this sodium silicate aqueous solution value with the condensation polymerization that carries out silicic acid.Then be cooled to 40 ℃, and to add concentration be the sodium aluminate aqueous solution 300ml of 10wt%, leave standstill made its reaction in 40 minutes after, once more by this Zeo-karb tubing string, and obtain the clarifying silicon dioxide gel A of an outward appearance.
This silicon dioxide gel A includes several through the sodium aluminate surfaction and include potassic silicon-dioxide polishing particles and aqueous medium, and described polishing particles (is made by moral Rui Ke (TREKINTAL) company through the nanometer particle size analyser, model is (MalvernHPPS)) detect after, show that described particle diameter is about 10～50nm.
Afterwards, with this silicon dioxide gel A, hexanodioic acid, anionic interfacial agent, benzotriazole, and hydrogen peroxide, mixed after taking off specified quantitative listed in the tabulation 1 respectively, and obtained the chemical and mechanical grinding fluid of embodiment 1-3.
The preparation of [comparative example 1-3] chemical and mechanical grinding fluid
The preparation method of similar embodiment 1-4, the chemical and mechanical grinding fluid of comparative example 1-3 is after making a silicon dioxide gel B earlier, with this silicon dioxide gel B, hexanodioic acid, anionic interfacial agent, benzotriazole, and hydrogen peroxide, take off tabulation respectively and mixed behind the listed specified quantitative in 1.
This silicon dioxide gel B prepares in the mode of similar above-mentioned silicon dioxide gel A, and its different place is to be, the alkalinisation treatment of this silicon dioxide gel B is that the NaOH aqueous solution with 5wt% carries out.This kind alkalinisation treatment also is the most normal tupe of selecting for use of present industry, and the silicon-dioxide polishing particles that is obtained is also through the sodium aluminate surfaction, and should include and contain sodium.
[test]
I. potassium content test--microwave-assisted acid digestion (this method is that the EPA, Executive Yuan in Taiwan announced on September 25th, 2000 in the Christian era, and its correlative detail sees also relevant bulletin { it is numbered No. the 55199th, (89) ring heat searching }):
This silicon dioxide gel A after high speed centrifugation and drying, is got silicon dioxide granule 0.1g wherein, and other gets the dense hydrofluoric acid mixing of 10ml, inserts microwave digestion device (microwave digestion equipment; Made by Perkin Elmer company, model be " 2000 "), obtain a solution after 10 minutes and shift out with 170 ℃ of reactions, then with induction coupled plasma mass spectrograph (inductive coupling plasma spectrometer, abbreviation IPC; Made by Agilent company, model is 7500C) come the small part of this solution is detected.
Ii. grind test--
Following examples and comparative example will grind test and analysis according to following condition and step:
1. test condition:
(1) instruments/equipment:
A. grinder station-(model is AMAT/Mirra for APPLIEDMATERIALS, INC.) manufacturing by limited-liability company of Applied Materials.
B. grinding pad (polishing pad)-by ROHM AND HAAS (Rohm﹠amp; Haas) company produces, and model is CUP4410.
C. the copper blank wafer-by Shanghai SMIC unicircuit Manufacturing Co., Ltd (SEMICONDUCTOR MANUFACTURING INTERNATIONALCORP.) manufacturing, thickness is 20000
D. the tantalum nitride blank wafer-by Shanghai SMIC unicircuit Manufacturing Co., Ltd (SEMICONDUCTOR MANU-FACTURING INTERNATIONALCORP.) manufacturing, thickness is 3000
E. the pattern wafer-for being coated with pattern (pattern) wafer (or be called " copper wafer ") of copper layer, by the manufacturing of U.S. Sematech company, live width is 0.18 μ m; The material of the barrier layer of this copper layer institute coating is a tantalum nitride.
(2) instrument is set:
Mould (membrane pressure) ... ... ..1.0～1.5psi
Original pressure (initial pressure) ... ... .1.5～2.0psi
Overdraft (down force pressure) ... 1.2～1.5psi
Interior pipe (inner tube) ... ... ... .... exhaust (vent)
Keep ring compression (retaining ring) ... ... 1.8psi
Grinding plate rotating speed (platen speed) ... .70rpm
Carrier rotating speed (carrier speed) ... ... ..74rpm
Temperature ... ... ... ... ... ... ... .25 ℃
Slurry flow rate ... ... ... ... ... ... ..200mL/min
2. test procedure:
Utilize above-mentioned grinder station respectively with each embodiment and comparative example, to a bronze medal blank wafer, tantalum nitride blank wafer, reach the copper pattern wafer and grind, and process of lapping is after this wafer is provided original pressure and lasts the grinding in 10 seconds, changes with overdraft mainly to grind; Grind the back and carry out the cleaning of wafer, and wafer is dried up with nitrogen with a cleaning machine (by the solid-state instrument company of the U.S. (Solid State Equipment Corporation) manufacturing, model is " EvergreenModel 10X ").Carry out following assessment at last again.
3. assessment:
(1) grinding rate: with the model of US business's KLA-Tencor company (KLA-TENCOR) manufacturing is that the thickness of KLA-Tencor RS-75 measures instrument (resistivitymeasurement system) and measures respectively and grind front and back copper blank wafer and the copper layer of tantalum nitride blank wafer and the thickness that tantalum nitride layer is removed, and knows this embodiment or the comparative example grinding rate for copper layer or tantalum nitride layer.Grinding rate be with 1 minute worn layer thickness
And define; The grinding rate of copper layer is preferable with 3000
More than be the acceptable scope of industry, the grinding rate value of tantalum nitride layer then is low more good more.
(2) marginal trough degree: with a contact-type surface profiler (SurfaceProfiler, model by US business's KLA-Tencor company (KLA-TENCOR) manufacturing is KLA-Tencor P-11), edge to crystal column surface measures, be gauge point with live width 100 μ m copper cash during mensuration, and measure the relative depression situation of this copper cash and a barrier layer (barrierlayer).Generally speaking, the numerical value of marginal trough degree is the smaller the better.
(3) surface observation of pattern wafer after grinding: utilize opticmicroscope (Optical Microscopy, an OM; Make by Olympus company, model is MX50A/T), with 1500 times enlargement ratios observe respectively each pattern wafer through the center of lapped face (center), the intermediate zone (middle) of edge (edge), center and edge, the polished situation of described barrier layer, and taken into optical microscopy map (being designated hereinafter simply as " OM figure ") and inspect, as Fig. 2,3 illustrated.The profile of each member has been black among Fig. 2, and the barrier layer of representing this place has been worn away and has manifested low dielectric material below it, is silicon-dioxide at this; The profile of reviewing each member among Fig. 3 is not black, and the barrier layer of representing this place is not by worn.
[result and discussion]
I. potassium content test--
Operation and test through " microwave-assisted acid digestion ", polishing particles among the silicon dioxide gel A will be converted into a solution and test its potassium content then, learn with the weight of described silicon dioxide granule sum total by test result and to calculate, potassium content in the colloidal sol of embodiment 1-3 in the particle is to account for 264ppm, and 4 of embodiment are to account for 212.4ppm.
As discussed previously, the difference of the embodiment of the invention and comparative example, should only be the silicon-dioxide polishing particles one that obtained for contain potassium another for containing sodium, in other words, if the embodiment grinding milk is with respect to each comparative example, really the advantage on the effect that shows is so it is former in pushing back due to " the silicon-dioxide polishing particles that contains potassium ".
Ii. grind test--
Chemical and mechanical grinding fluid with embodiment 1-4 and comparative example 1-3, test according to above-mentioned grinding test mode and analytical procedure respectively, described result is composition characteristic, each composition proportion of the grinding milk of described embodiment, comparative example etc., and one is listed in following table 1.The concentration of each composition or ratio are to be foundation with " weight ", and " Gu composition " represents the content of silicon dioxide granule; And just " surface observation behind the pattern grinding wafer " one respectively with the described OM figure result of each symbolic representation." zero " represents that this profile of locating each member is not black, that is to say, by excessively worn (no tantalum nitride barrier layer infringement), pairing OM figure is not as shown in Figure 3 for its barrier layer; " * " represents that this profile of locating each member obviously is black, that is to say, by excessively worn (infringement of tantalum nitride barrier layer is arranged), pairing OM figure as shown in Figure 2 significantly for its barrier layer; " △ " represents that this profile of locating each member is black slightly, that is to say, its barrier layer has the excessively worn phenomenon of slight quilt (slight tantalum nitride barrier layer infringement).
Table 1
Now classify with the embodiment of solid composition unanimity and comparative example and be compared as follows.
[the effect discussion of each chemical and mechanical grinding fluid]
(1) embodiment 1 and comparative example 1
Pattern crystal column surface after grinding with embodiment 1 grinding milk, no matter be heart place, edge therein, or intermediate zone, each member profile all is not black, the barrier layer (TaN) of the pattern wafer that is obviously ground does not all have over-lapping and exposes beneath SiO
2Layer, this represents that promptly embodiment 1 slurry also can effectively avoid the barrier layer over-lapping, has met the expectation of industry to fs chemomechanical copper grinding slurries.
Review the pattern crystal column surface after grinding with comparative example 1 grinding milk, find heart place, edge therein, or intermediate zone, each member profile has been black all, shows that the pattern wafer that comparative example 1 grinding milk can't be avoided being ground produces the infringement of tantalum nitride barrier layer.
Other sees Table the embodiment 1 shown in 1 and the efficacy data of comparative example 1 each grinding milk, obvious with regard to copper grinding rate (data of embodiment 1 are greater than comparative example 1), tantalum nitride grinding rate (embodiment 1 only be comparative example 1 40%), and aspect such as marginal trough degree (embodiment 1 only be comparative example 1 63%), embodiment 1 all has better effect than comparative example 1.
Based on the above results, can seem the overall efficacy of embodiment 1, the comparative example 1 that is better than industry approval use is a lot of, and more can meet the demand of industry.
(2) embodiment 2 and comparative example 2
Pattern crystal column surface after grinding with embodiment 2 grinding milks, all little black that is of member profile throughout, the therefore barrier layer (TaN) of the pattern wafer that is ground, existing a little denuded, avoided the infringement of part tantalum nitride barrier layer to produce.
Review the pattern crystal column surface after grinding with comparative example 2 grinding milks, find that member profile throughout has been black all, show that the pattern wafer that comparative example 2 grinding milks can't be avoided being ground fully produces the infringement of tantalum nitride barrier layer; Therefore embodiment 2 grinding milks more can be avoided the barrier layer over-lapping of pattern wafer with respect to comparative example 2.
Other sees Table the embodiment 2 shown in 1 and the efficacy data of comparative example 2 each grinding milk, obvious with regard to copper grinding rate (embodiment 2 only lower slightly comparative example 2 a little), tantalum nitride grinding rate (embodiment 2 only be comparative example 2 45%), and aspect such as marginal trough degree (embodiment 2 only be comparative example 2 50.85%), embodiment 2 also has good performance.
Based on the above results, can seem the overall efficacy of embodiment 2, be better than the comparative example 2 that the industry approval is used, and more can meet the demand of industry.
(3) embodiment 3,4 and comparative example 3
Pattern crystal column surface after grinding with embodiment 3,4 grinding milks, member profile everywhere all is not black, and the barrier layer (TaN) of the obvious pattern wafer that grinds does not all have over-lapping and exposes beneath SiO
2Layer, this represents that promptly embodiment 3,4 can effectively avoid the barrier layer over-lapping of pattern wafer, has met the expectation of industry to fs chemomechanical copper grinding slurries.
Review the pattern crystal column surface after grinding with comparative example 3 grinding milks, find that member profile throughout has been black all, show that comparative example 3 grinding milks are the same with comparative example 1,2, the pattern wafer that can't avoid completely being ground produces the infringement of tantalum nitride barrier layer; Therefore embodiment 3,4 grinding milks more can be avoided the barrier layer over-lapping of pattern wafer with respect to comparative example 3.
Other sees Table the embodiment 3 shown in 1 and the efficacy data of comparative example 3 each grinding milk, obvious with regard to copper grinding rate (embodiment 3 is higher than comparative example 3), tantalum nitride grinding rate (embodiment 3 only for comparative example 3 20.66%), and the marginal trough degree (embodiment 3 shows 752
The high level of/100 μ m, only be comparative example 3 48.80%) etc. the aspect, embodiment 3 all shows excellent effect.And embodiment 4 aspects, the tantalum nitride grinding rate only has 13.22% of comparative example 3, and the marginal trough degree then is 774
/ 100 μ m are 50.23% of comparative example 3, so embodiment 4 performance in every respect is also very outstanding.
Based on the above results, can seem the overall efficacy of embodiment 3,4, the comparative example 3 that is better than industry approval use is a lot, and more can meet the demand of industry.
By the result of above each embodiment and comparative example as seen, each embodiment grinding milk the corresponding crystal column surface that grinds, almost all show lower TaN grinding rate, higher copper grinding rate, and lower marginal trough degree; Demonstrate with regard to the observations of OM figure in addition and be subjected to described embodiment grinding milk with respect to each comparative example, the crystal column surface that more can avoid effectively being ground produces the infringement of tantalum nitride barrier layer.
And not the existing together of each embodiment grinding milk and pairing comparative example, it only is the silicon-dioxide polishing particles that is that it is contained, be in processing procedure, to carry out the condensation polymerization reaction respectively, cause both structural difference with the KOH aqueous solution or the general NaOH aqueous solution commonly used.Comparison by their effects, confirmation contains several through an aluminium surfaction and include the chemical and mechanical grinding fluid of the silicon-dioxide polishing particles of potassium by of the present invention, except the general chemical and mechanical grinding fluid of certain ratio, the wafer that more can avoid being ground produces beyond the infringement of tantalum nitride barrier layer, very excellent performance is also all arranged on other each professional test, meet very much pressing for of present industry.
Claims (19)
1. a chemical and mechanical grinding fluid comprises: a kind of acid, a kind of interfacial agent, and a kind of aqueous medium; It is characterized in that, this chemical and mechanical grinding fluid also comprises several and carries out surfaction through a kind of surface electrical behavior modification agent, and potassic silicon-dioxide polishing particles, described silicon-dioxide polishing particles is via after an aqueous silicate solution being carried out one decationizing processing, carry out condensation polymerization reaction with potassium hydroxide or potash water glass, carried out one decationizing then behind the surfaction again and handle and obtain.
2. chemical and mechanical grinding fluid according to claim 1 is characterized in that, this surface electrical behavior modification agent is an aluminate.
3. chemical and mechanical grinding fluid according to claim 2 is characterized in that, this surface electrical behavior modification agent is sodium aluminate or potassium aluminate.
4. chemical and mechanical grinding fluid according to claim 1 is characterized in that, in the gross weight of described silicon-dioxide polishing particles, the content of potassium is to account for more than the 100ppm.
5. chemical and mechanical grinding fluid according to claim 1 is characterized in that, in the gross weight of described silicon-dioxide polishing particles, the content of potassium is to account for more than the 200ppm.
6. chemical and mechanical grinding fluid according to claim 1 is characterized in that, its pH value is between 2～5.
7. chemical and mechanical grinding fluid according to claim 6 is characterized in that, its pH value is between 3～4.
8. chemical and mechanical grinding fluid according to claim 1, it is characterized in that, this acid is propanedioic acid, Succinic Acid, pentanedioic acid, hexanodioic acid, vinylformic acid, the 2-oxyacetic acid, formic acid, acetate, caproic acid, lactic acid, oxysuccinic acid, tartrate, glyconic acid, citric acid, hydrochloric acid, sulfuric acid, maleic acid, FUMARIC ACID TECH GRADE, 2, the 2-dimethyl succinic acid, 2-ethyl-2-pyrovinic acid, 2, the 3-dimethyl succinic acid, the methyne Succinic Acid, 2-methyl-maleic acid, 2-methyl-FUMARIC ACID TECH GRADE, 2-methyl-2-oxyacetic acid, 2-ethyl-2-oxyacetic acid, 2,2-diethyl-2-oxyacetic acid, 2-ethyl-2-methyl-2-oxyacetic acid, the 2-methacrylic acid, the 2-ethylacrylic acid, the 3-methacrylic acid, 2, the 3-dimethacrylate, 1,2,3,4-BTCA, or these a combination.
9. chemical and mechanical grinding fluid according to claim 8 is characterized in that, this acid is Succinic Acid, pentanedioic acid, hexanodioic acid, methyne Succinic Acid, FUMARIC ACID TECH GRADE, vinylformic acid, 2-oxyacetic acid, formic acid, 1,2,3,4-BTCA, or these a combination.
10. chemical and mechanical grinding fluid according to claim 9 is characterized in that this acid is hexanodioic acid, or hexanodioic acid, methyne Succinic Acid, formic acid, with 1,2,3, and a combination of 4-BTCA.
11. chemical and mechanical grinding fluid according to claim 1 is characterized in that, this interfacial agent is anionic interfacial agent or non-ionic interfacial agent.
12. chemical and mechanical grinding fluid according to claim 1 is characterized in that, also comprises to select certainly in the additive of following group: fungistat, corrosion inhibitor, oxygenant, stablizer, and these a combination.
13. chemical and mechanical grinding fluid according to claim 12 is characterized in that, also comprises a corrosion inhibitor.
14. chemical and mechanical grinding fluid according to claim 13 is characterized in that, this corrosion inhibitor is to be selected from the group that is made of following: benzotriazole, tricyanic acid, 1,2,3-triazole, 3-amido-1,2,4-triazole, 3-nitro-1,2,4-triazole, 4-amido-3-diazanyl-1,2,4-triazolyl-5-mercaptan, benzotriazole-5-carboxylic acid, 3-amido-1,2,4-triazole-5-carboxylic acid, I-hydroxybenzotriazole, nitrobenzene and triazolam, and these a combination.
15. chemical and mechanical grinding fluid according to claim 14 is characterized in that, this corrosion inhibitor is a benzotriazole.
16. chemical and mechanical grinding fluid according to claim 12 is characterized in that, also comprises an oxygenant.
17. chemical and mechanical grinding fluid according to claim 16 is characterized in that, this oxygenant is to be selected from the group that is made of following: hydrogen peroxide, iron nitrate, Potassium Iodate, peracetic acid, potassium permanganate, and these a combination.
18. chemical and mechanical grinding fluid according to claim 17 is characterized in that, this oxygenant is a hydrogen peroxide.
19. a chemical mechanical planarization method comprises the following step: a wafer is contacted with a grinding pad; (B) carry one to have the chemical and mechanical grinding fluid of several silicon-dioxide polishing particles to this wafer and grinding pad; And (C) with this chemical and mechanical grinding fluid with the surface of this wafer to the small part planarization; It is characterized in that: described silicon-dioxide polishing particles is to carry out surfaction through a kind of surface electrical behavior modification agent, and contain potassium, described silicon-dioxide polishing particles is via after an aqueous silicate solution being carried out one decationizing processing, carry out condensation polymerization reaction with potassium hydroxide or potash water glass, carried out one decationizing then behind the surfaction again and handle and obtain.
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| CN1357585A (en) * | 2000-12-04 | 2002-07-10 | 拜尔公司 | Chemical and mechanical polishing paste for metal and dielectric structure |
| CN1428388A (en) * | 2001-12-27 | 2003-07-09 | 拜尔公司 | Composition for chemical mechanical polishing of metal and metal/electric medium structure |
| CN1543491A (en) * | 2001-06-14 | 2004-11-03 | PPG��ҵ����˾ | Silica-based slurry |
| US20050112892A1 (en) * | 2003-11-20 | 2005-05-26 | Eternal Chemical Co., Ltd. | Chemical mechanical abrasive slurry and method of using the same |
| WO2006133249A2 (en) * | 2005-06-06 | 2006-12-14 | Advanced Technology Materials, Inc. | Integrated chemical mechanical polishing composition and process for single platen processing |
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| CN1357585A (en) * | 2000-12-04 | 2002-07-10 | 拜尔公司 | Chemical and mechanical polishing paste for metal and dielectric structure |
| CN1543491A (en) * | 2001-06-14 | 2004-11-03 | PPG��ҵ����˾ | Silica-based slurry |
| CN1428388A (en) * | 2001-12-27 | 2003-07-09 | 拜尔公司 | Composition for chemical mechanical polishing of metal and metal/electric medium structure |
| US20050112892A1 (en) * | 2003-11-20 | 2005-05-26 | Eternal Chemical Co., Ltd. | Chemical mechanical abrasive slurry and method of using the same |
| WO2006133249A2 (en) * | 2005-06-06 | 2006-12-14 | Advanced Technology Materials, Inc. | Integrated chemical mechanical polishing composition and process for single platen processing |
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