CN102888208A - Abrasive and substrate polishing method - Google Patents

Abrasive and substrate polishing method Download PDF

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Publication number
CN102888208A
CN102888208A CN2012102534790A CN201210253479A CN102888208A CN 102888208 A CN102888208 A CN 102888208A CN 2012102534790 A CN2012102534790 A CN 2012102534790A CN 201210253479 A CN201210253479 A CN 201210253479A CN 102888208 A CN102888208 A CN 102888208A
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abrasive
layer
compound
cobalt
metal
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CN2012102534790A
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CN102888208B (en
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三嶋公二
飞田文子
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Lishennoco Co ltd
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Hitachi Chemical Co Ltd
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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
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1409—Abrasive particles per se
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00—Brightening metals by chemical means
    • C23F3/04—Heavy metals
    • C23F3/06—Heavy metals with acidic solutions
    • 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

Abstract

The invention provides an abrasive for polishing cobalt-containing layers. The abrasive comprises a carboxylic acid derivative, a metal corrosion inhibitor and water, the carboxylic acid derivative consisting of at least one selected from a phthalic compound, an isophthalic compound, an alkyl dicarboxylic compound represented by the formula (I), and salts and anhydrides of the phthalic compound, the isophthalic compound and the alkyl dicarboxylic compound. The pH is below 4.0. Formula (I): HOOC-R-COOH.

Description

The Ginding process of abrasive and substrate
Technical field
The present invention relates to the Ginding process of abrasive and substrate.
Background technology
In recent years, be accompanied by semiconductor integrated circuit (below be designated as " LSI ".) Highgrade integration, high performance, developed new Micrometer-Nanometer Processing Technology.Cmp (below be designated as " CMP ".) method also is wherein a kind of, is the technology of frequent utilization in the planarization that forms the isolator in the operation of LSI manufacturing process, especially multilayer wiring, metallic plug formations, the embedded wiring formation etc.
In addition, in order to make the LSI high performance, attempting utilizing copper alloy as wiring material recently.But copper alloy is difficult to carry out the microfabrication of the frequent dry etching method that uses in based on the formation of in the past aluminium alloy wiring.Therefore, for example, mainly adopt so-called inlaying (damascene) method, pile up, embed copper alloy thin films at the insulating film that is pre-formed groove, remove slot part copper alloy thin films in addition by CMP, form embedded wiring (for example, with reference to patent documentation 1.）。
The general method of the CMP of metal is, grinding plate (Platen) in circle is pasted abrasive cloth, the surface of abrasive cloth is infiltrated with abrasive with liquid metal, presses the face of the metallic membrane that forms substrate, with the pressure that applies regulation from the back side (below be designated as " grinding pressure ".) state rotate grinding plate, with the mechanical friction between the protuberance of abrasive and metallic membrane, remove the metallic membrane of protuberance by metal.
The metal that uses among the CMP generally contains oxygenant and abrasive particle with abrasive, further adds as required dissolving metal agent, corrosion inhibitor for metal etc.When adding these, think that basic mechanism is with film surface, dissolving metal agent oxidized metal, scrapes off zone of oxidation with abrasive particle.Think to contact the zone of oxidation of the metallic film surface that becomes recess hardly with abrasive cloth, do not reach and be polished the effect that abrasive particle scrapes off, therefore be accompanied by the carrying out of CMP, the metal level of protuberance is removed, the substrate surface planarization.
On the other hand, shown in Fig. 1 (a), in the lower floor of the conductive material layer 5 that is formed with metal by the wiring of copper or copper alloy etc., in order to prevent the diffusion in the isolator 2 that copper forms on the silicon substrate 1 and to improve adaptation, and form below the barrier metal electrically conductive film 3(, be also referred to as " barrier metal layer 3 ").Thereby embedded wiring need to be removed by CMP with the barrier metal layer that exposes 3 beyond the wiring section of metal.
Therefore, general applicable two sections Ginding process, namely be divided into from the state shown in Fig. 1 (a) to the state shown in Fig. 1 (b) " the 1st grinding step " that grind conductive material layer 5 with, from the state shown in Fig. 1 (b) to the state shown in Fig. 1 (c) " the 2nd grinding step " of grinding barrier metal layer 3, grind with different abrasives respectively.
, along with the miniaturization of design rule, each layer that above-mentioned wiring forms operation also tends to attenuation.Yet, because above-mentioned barrier metal layer 3 attenuation prevent from containing the diffusion effect that for example is selected from least a kind conductive material in copper or copper alloy and their oxide compound and just reduce.In addition, because wiring width narrows down, the imbedibility of conductive material reduces, and wiring section produces the emptying aperture that is called void.The tendency that reduction is also arranged with the adaptation of conductive material layer further.Therefore, the metal that will be in the barrier metal layer 3 among Fig. 1 uses of research replaces to and contains the Co(cobalt) metal of element.In addition, suggestion makes the metal level that contains cobalt element (below, be also referred to as " cobalt layer 4 ") every between barrier metal layer 3 and conductive material layer 5 shown in Fig. 2 (a).By using cobalt layer 4, not only suppressed the diffusion of conductive material, and because cobalt and high as the affinity between the widely used copper of conductive material, so the copper layer can further remedy the adaptation with the copper layer in the imbedibility raising of wiring section.
When using cobalt as barrier metal layer, need metal to remove unnecessary cobalt layer with abrasive.Known many kinds of substance is as the metal abrasive, and on the other hand, when having certain metal to use abrasive, it differs and removes surely arbitrarily metal.As metal abrasive in the past, known metal with copper, tantalum, titanium, tungsten, aluminium etc. is as grinding object (removing the object of redundance), but also not too knows with cobalt as the abrasive that grinds object.
Yet, because cobalt and the conductive material that was used as copper that wiring uses with metal etc. are relatively in the past, corrodibility is strong, if therefore directly use abrasive in the past, cobalt is just by excessive erosion (etching), or in wiring layer, produce slit, and therefore can not play the function as barrier metal layer, the possibility of metal ion diffusion is arranged.When metal ion spread in the isolator, the possibility of semiconducter device short circuit uprised.On the other hand, if prevent such thing, add the strong inhibitor of corrosion-resisting function, or increase the addition of inhibitor, the problem that reduces whole grinding rate is then arranged.
For such problem, the abrasive of the specific corrosion inhibitor for metal of known use, this corrosion inhibitor for metal is the heterogeneous ring compound of tetra-atomic ring ~ six-ring, contains the two keys more than 2, contains nitrogen-atoms more than 1 (for example, with reference to patent documentation 2.）。According to such abrasive, in the time of the protection wiring layer, can prevent that slit is arranged in the wiring layer.
Prior art
Patent documentation
Patent documentation 1: Japanese patent laid-open 2-278822 communique
Patent documentation 2: Japanese Patent Laid-Open 2011-91248 communique
Summary of the invention
The problem that invention will solve
Yet, only rely on the effect of corrosion inhibitor for metal, although can suppress the etching of cobalt, be not easy to keep simultaneously the high grinding rate for cobalt, seek more to improve the grinding rate to cobalt.The present invention wants to solve above-mentioned problem, and purpose suppresses cobalt layer burn into and suppresses the abrasive that slit produces and the substrate Ginding process that uses this abrasive when being to provide the good grinding rate that keeps the cobalt layer.
Solve the means of problem
In order to solve so wholwe-hearted result of study of problem in the past, the inventor finds, by using specific carboxylic acid derivative, when can keep the good grinding rate to the cobalt layer, the corrosion-inhibiting of cobalt layer is excellent, suppresses the generation of slit.
The concrete method that solves above-mentioned problem is as described below.
＜1＞a kind of abrasive, be used for grinding the layer that contains cobalt element, it contains by being selected from phthalic compounds, m-phthalic acid compound and alkyl dicarboxylic aid's compound of following general formula (I) expression and carboxylic acid derivative, corrosion inhibitor for metal and the water of at least a formation in their salt and the acid anhydrides, and the pH of abrasive is below 4.0.
HOOC-R-COOH…(I)
(in the above-mentioned general formula (I), R represents that carbonatoms is 4 ~ 10 alkylidene group.）
By being set as such abrasive, when can keep the good grinding rate for the cobalt layer, improve corrosion-inhibiting.
＜2＞a kind of abrasive, be used for grinding the layer that contains cobalt element, it contains by at least a above carboxylic acid derivative, corrosion inhibitor for metal and water in the alkyl dicarboxylic aid's compound that is selected from phthalic compounds, m-phthalic acid compound and following general formula (I) expression and their salt and the acid anhydrides, the pH of abrasive is below 4.0, in 50 ℃ abrasive for the etching speed of cobalt below 10.0nm/min.
HOOC-R-COOH…(I)
(in the above-mentioned general formula (I), R represents that carbonatoms is 4 ~ 10 alkylidene group.）
By being set as such abrasive, when can keep the good grinding rate for the cobalt layer, improve corrosion-inhibiting.
＜3＞described＜1〉or＜2 described in abrasive, described corrosion inhibitor for metal contains the compound with triazole skeleton.
Thus, can more effectively suppress corrodibility.
＜4＞above-mentioned＜1＞~＜3＞in the described abrasive of any one, further contain oxygenant.
Thus, when being polished film and containing layer beyond the cobalt layer, can more improve the grinding rate of the layer beyond the cobalt layer.
＜5＞described＜1＞~＜4＞in the described abrasive of any one, further contain organic solvent.
Thus, when being polished film and containing layer beyond the cobalt layer, owing to improving for the wettability of the layer beyond the cobalt layer, therefore can more improve grinding rate.
＜6＞described＜1＞~＜5＞in the described abrasive of any one, further contain water-soluble polymers.
Thus, protection is polished face, suppresses corrosion, can reduce the generation of the defective of wound etc.
＜7＞described＜1＞~＜6＞in the described abrasive of any one, further contain abrasive particle.
Thus, when being polished film and containing layer beyond the cobalt layer, can more improve the grinding rate of the layer beyond the cobalt layer.
＜8＞a kind of removal contains the substrate Ginding process of the redundance of cobalt element, uses described＜1〉~＜7 in the described abrasive of any one grind the film that is polished that contains cobalt element that forms at least one surface of substrate.
According to Ginding process of the present invention, can at a high speed and suppress excessive corrosion ground and grind the film that is polished that contains cobalt element.
The effect of invention
According to the present invention, the abrasive of the corrosion-inhibiting excellence of cobalt layer and the substrate Ginding process that uses it when the good grinding rate of a kind of maintenance to the cobalt layer can be provided.
Description of drawings
Fig. 1 is the pattern sectional view of the cloth wire forming proces in the mosaic procedure that shows in the past.
Fig. 2 is the pattern sectional view that shows the cloth wire forming proces in the mosaic procedure that uses the cobalt layer.
Fig. 3 is the sectional view that shows with an example of the substrate after the Ginding process grinding of the present invention.
Nomenclature
1 silicon substrate
2 isolators
3 barrier metal layers
4 cobalt layers
5 conductive material layers (wiring metal)
Embodiment
Word in this specification sheets " operation " is not only operation independently, even in the time of can not clearly distinguishing with other operation, as long as reach the desired purpose of its operation, just be included in this word.Use in addition the numerical range of "～" expression, the numerical value that represents the front and back of " ~ " are put down in writing is respectively as minimum value and the contained scope of maximum value.The content of each composition in the abrasive further when having a plurality of material that is equivalent to each composition in abrasive, except as otherwise noted, means total metering of these a plurality of materials that exist in the abrasive.
Below, to of the present invention for grinding contain cobalt element the layer abrasive (below, only be called " abrasive ".) and the suitable embodiment of substrate Ginding process be elaborated.
[abrasive]
Abrasive of the present invention contains by being selected from phthalic compounds, m-phthalic acid compound and alkyl dicarboxylic aid's compound of following general formula (I) expression and carboxylic acid derivative, corrosion inhibitor for metal and the water of at least a formation in their salt and the acid anhydrides, and pH is below 4.0.
HOOC-R-COOH…(I)
(in the above-mentioned general formula (I), R represents that carbonatoms is 4 ~ 10 alkylidene group.）
＜carboxylic acid derivative＞
Abrasive of the present invention contains dicarboxylic acid compound (being " specific dicarboxylic acid compound " hereinafter referred to as them) and their salt and at least a carboxylic acid derivative in the acid anhydrides (hereinafter referred to as " specific carboxylic acid derivative ") that is selected from phthalic compounds, m-phthalic acid compound and following general formula (I) expression.Above-mentioned specific carboxylic acid derivative can a kind of independent use, perhaps two or more mixing uses.By the above-mentioned specific carboxylic acid derivative of from the carboxylic acid of countless existence and carboxylic acid derivative, selecting, can in the good grinding rate that keeps the cobalt layer, moderately control etching speed, suppress corrosion, obtain good abrasive surface.Even further under harsher condition (for example 50 ℃), the etching speed of cobalt layer is also more effectively suppressed, and can reach excellent corrosion-inhibiting.The corrosion-inhibiting excellence comprises herein: be polished on the face, effectively suppress the cobalt layer etched, or produce slit in the wiring layer.
The reason that obtains such effect is also unclear, and the inventor is following to infer.That is, think above-mentioned specific carboxylic acid derivative, for example have as dissolving metal agent work, improve the effect to the grinding rate of cobalt layer.Infer that above-mentioned specific carboxylic acid derivative has such function simultaneously, by two carboxyls and cobalt atom chelating structure circlewise, control etching speed in order to form stable complex compound state, have the function that suppresses to be polished the corrosion in the face.The in addition formation of this stable complex status may also be of value to corrosion inhibitor for metal described later.
Consider from the viewpoint to the controlled and corrosion-inhibiting of the grinding rate of cobalt layer, etching speed, above-mentioned specific carboxylic acid derivative from dicarboxylic acid compound, they salt and their acid anhydrides select.Acidic cpd beyond the above-mentioned specific carboxylic acid derivative is difficult to two vertical sometimes to the good grinding rate of cobalt layer and the etching speed that suppresses the cobalt layer.Think that this is that the three-dimensional arrangement of acidic cpd becomes important factor because the formation of stable complex status described above is important.In addition, even contain above-mentioned specific carboxylic acid derivative, if contain in addition other acidic cpd, the etching speed of cobalt layer significantly rises sometimes.Think that this is because the effect of other acidic cpd etching cobalt layer has precedence over the formation of aforesaid complex status.
The first form of the present invention is, above-mentioned carboxylic acid derivative is by the alkyl dicarboxylic aid's compound that is selected from phthalic compounds, m-phthalic acid compound and above-mentioned general formula (I) expression and at least a formation in their salt and the acid anhydrides.But, above-mentioned carboxylic acid derivative is in the scope of significantly not damaging effect of the present invention, can comprise other carboxylic acid derivative, its be selected from dicarboxylic acid compound beyond alkyl dicarboxylic aid's compound of phthalic compounds, m-phthalic acid compound and above-mentioned general formula (I) expression, and they salt and their acid anhydrides at least a.Namely, above-mentioned carboxylic acid derivative is, by the alkyl dicarboxylic aid's compound that is selected from phthalic compounds, m-phthalic acid compound and above-mentioned general formula (I) expression and material that at least a specific carboxylic acid derivative in their salt and the acid anhydrides substantially consists of." substantially " herein refers to significantly not damage the scope of effect of the present invention, and particularly, the containing ratio that means above-mentioned other carboxylic acid derivative is below the 10 quality % with respect to the total mass of specific carboxylic acid derivative.The containing ratio of above-mentioned other carboxylic acid derivative is further below the preferred 5 quality %, more preferably below the 1 quality %.
Same viewpoint, the second form of abrasive of the present invention is, above-mentioned carboxylic acid derivative contains: be selected from least a in alkyl dicarboxylic aid's compound of phthalic compounds, m-phthalic acid compound and above-mentioned general formula (I) expression and their salt and the acid anhydrides, in 50 ℃ abrasive for the etching speed of cobalt below 10.0nm/min.In the second form, above-mentioned carboxylic acid derivative can contain other carboxylic acid derivative, these other carboxylic acid derivative be selected from dicarboxylic acid compound beyond alkyl dicarboxylic aid's compound of phthalic compounds, m-phthalic acid compound and above-mentioned general formula (I) expression, and they salt and their acid anhydrides at least a, but need in 50 ℃ abrasive, be no more than 10.0nm/min about the preferable range of the containing ratio of above-mentioned other carboxylic acid derivative by the etching speed for cobalt, with above-mentioned the first homomorphosis.
Etching speed for cobalt in 50 ℃ abrasive can be as measuring as following.Namely, formed the square chip (estimate and use chip) of 20mm of the cobalt layer of 0.3 μ m on the prepared silicon substrate, in the beaker that adds the 50g abrasive, put into above-mentioned evaluation chip, be immersed in 50 ℃ the thermostatic bath 1 minute, by measuring the film thickness of the cobalt layer before and after soaking, as (thickness of the cobalt layer after the thickness of the cobalt layer before soaking-immersion)/[nm/min] tried to achieve in 1 minute.
In the second form of abrasive of the present invention, above-mentioned etching speed is considered from the viewpoint that improves better corrosion-inhibiting below 10.0nm/min, below the preferred 9.0nm/min, more preferably below the 8.0nm/min.
In the first form of abrasive of the present invention, also to consider from the viewpoint that more improves corrosion-inhibiting, above-mentioned etching speed is preferably below 10.0nm/min, more preferably below the 9.0nm/min, below the further preferred 8.0nm/min.
In the above-mentioned specific dicarboxylic acid compound, comprise in the phthalic compounds that at least a kind of more than one substituent phthalic acid derivatives is arranged on phthalic acid (benzene-1,2-dicarboxylic acid) and the phenyl ring.Described substituting group is for example such as methyl, amino, nitro etc.Wherein, at least one in preferred nitro and the methyl, more preferably nitro.
As above-mentioned phthalic compounds, can enumerate particularly the alkyl phthalic acid of phthalic acid, 3-methylphthalic acid, 4-methylphthalic acid etc.; The aminophthalic acid of 3-aminophthalic acid, 4-aminophthalic acid etc.; The nitrophthalic acid of 3-nitrophthalic acid, 4-nitrophthalic acid etc. etc.Wherein, preferably contain nitro as substituent phthalic compounds (nitrophthalic acid), more preferably at least one in 3-nitrophthalic acid and the 4-nitrophthalic acid, particularly preferably 3-nitrophthalic acid.Above-mentioned phthalic compounds can be used with anhydride form, also can use with the form of salt.
In the above-mentioned m-phthalic acid compound, comprise at least a kind that has on m-phthalic acid (benzene-1,3-dicarboxylic acid) and the phenyl ring in the more than one substituent isophthalic acid derivatives.Above-mentioned substituting group is for example such as nitro, methyl, amino, hydroxyl etc.Wherein, preferred nitro.
Above-mentioned m-phthalic acid compound, specifically can enumerate as, m-phthalic acid, 5-nitroisophthalic acid etc.Above-mentioned m-phthalic acid compound can use salt form.
Alkyl dicarboxylic aid's compound of above-mentioned general formula (I) expression can be the alkyl dicarboxylic aid's compound with alkylidene group of carbonatoms 4 ~ 10.Moreover above-mentioned carbonatoms is the carbonatoms of alkylidene group, and the carbon atom that comprises in the carboxyl not can be regarded as described carbonatoms.Above-mentioned alkylidene group can be any in ring-type, straight chain shape and the chain.Wherein, preferred straight chain shape.To the grinding rate of cobalt layer, to consider from the controlled and corrosion inhibition viewpoint of etching speed, preferred carbonatoms is 4 ~ 8, more preferably carbonatoms is 4 ~ 6.
As the alkyl dicarboxylic aid of the alkylidene group with carbonatoms 4 ~ 10, specifically can enumerate hexanodioic acid, pimelic acid, suberic acid, nonane diacid etc.Wherein, preferred hexanodioic acid, pimelic acid, more preferably pimelic acid.
Take the total mass of abrasive as benchmark, the content of above-mentioned carboxylic acid derivative is preferably in the scope of 0.001 quality % ~ 10 quality %.Adjust to above-mentioned scope by the content of above-mentioned carboxylic acid derivative, can obtain near the good grinding rate of the cobalt layer that arranges of cobalt layer layer (wiring of the copper of the conductive material layer 5 that for example, represents among Fig. 2 (a) etc. metal or barrier metal layer 3 etc.) in addition.
Consider from the viewpoint of grinding rate, the content of above-mentioned carboxylic acid derivative is more preferably more than the 0.01 quality %, further more than the preferred 0.03 quality %, particularly preferably more than the 0.05 quality %.In addition, consider from the viewpoint to the etching inhibition of cobalt layer and corrosion-inhibiting, below the preferred 5.0 quality % of the content of above-mentioned dicarboxylic acid, more preferably below the 3.0 quality %, further below the preferred 1.0 quality %, very preferably below the 0.7 quality %, below the extremely preferred 0.5 quality %.
Above-mentioned abrasive, consider from the viewpoint of grinding rate, preferably contain being selected from alkyl phthalic acid, aminophthalic acid, nitrophthalic acid, m-phthalic acid, 5-nitroisophthalic acid and being at least a in alkyl dicarboxylic aid's compound of straight chain shape alkylidene group of carbonatoms 4 ~ 8 and their salt and the acid anhydrides as general formula (I) expression, R more than the 0.01 quality % as carboxylic acid derivative.
In addition above-mentioned abrasive, from suppressing the viewpoint consideration to the etch effect of cobalt layer, as carboxylic acid derivative, preferably contain 5.0 quality % following be selected from alkyl phthalic acid, aminophthalic acid, nitrophthalic acid, m-phthalic acid, 5-nitroisophthalic acid and general formula (I) expression, R is alkyl dicarboxylic aid's compound of the straight chain shape alkylidene group of carbonatoms 4 ~ 8, and at least a in their salt and the acid anhydrides.
＜corrosion inhibitor for metal＞
The corrosion inhibitor for metal that comprises in the abrasive of the present invention has no particular limits, and in the past known conduct has the compound of corrosion-resisting function to use to metal.Particularly, can use and be selected from least a in triazole compounds, pyridine compounds, pyrazole compound, pyrimidine compound, imidazolium compounds, guanidine compound, thiazolium compounds, tetrazole compound, triaizine compounds, the vulkacit H." compound " herein refers to have the general name of the compound of its skeleton, and for example triazole compounds refers to have the compound of triazole skeleton.
Triazole compounds can enumerate as; 1; 2; the 3-triazole; 1; 2; the 4-triazole; 3-amino-1H-1,2,4-triazole; benzotriazole; I-hydroxybenzotriazole; 1-dihydroxypropyl benzotriazole; 2; 3-dicarboxyl propyl group benzotriazole; the 4-hydroxybenzotriazole; 4-carboxyl-1H-benzotriazole; 4-carboxyl-1H-benzotriazole methyl esters (1H-benzotriazole-4-carboxylate methyl ester); 4-carboxyl-1H-benzotriazole butyl ester (1H-benzotriazole-4-butyl carboxylate); 4-carboxyl-1H-benzotriazole monooctyl ester (1H-benzotriazole-4-carboxylic acid monooctyl ester); 5-hexyl benzotriazole; (1; 2,3-benzotriazole-1-methyl) (1,2; 4-benzotriazole-1-methyl) (2-ethylhexyl) amine; tolyl-triazole; aphthotriazoles; two [(1-benzotriazole base) methyl] phosphonic acids; 3H-1; 2,3-triazolo [4,5-b] pyridine-3-alcohol; 1H-1; 2; 3-triazolo [4,5-b] pyridine; 1-ethanoyl-1H-1,2; 3-triazolo [4; 5-b] pyridine; the 3-pyridone; 1,2,4-triazolo [1; 5-a] pyrimidine; 1; 3,4,6; 7; 8-six hydrogen-2H-Kui Linpyrimido quinoline [1,2-a] pyrimidine; 2-methyl-5,7-phenylbenzene-[1; 2; 4] triazolo [1,5-a] pyrimidine; 2-sulfonyloxy methyl-5,7-phenylbenzene-[1; 2; 4] triazolo [1,5-a] pyrimidine; 2-sulfonyloxy methyl-5,7-phenylbenzene-4; 7-dihydro-[1; 2,4] triazolo [1,5-a] pyrimidine etc.Moreover, when having triazole skeleton and skeleton in addition in a part, be categorized as triazole compounds.
As pyridine compounds, can give an example as, oxine, Protionamide, 2-nitropyridine-3-alcohol, Pyridoxylamine, nicotinamide, iproniazid (Iproniazid), γ-picolinic acid, benzo [f] quinoline, 2,5-Pyridinedicarboxylic acid, 4-stibazole, neonicotine, 4-nitropyridine-1-oxide compound, pyridine-3-vinyl acetic monomer, quinoline, 2-ethylpyridine, quinolinic acid, methylarecaidin, citrazinic acid, pyridine-3-methyl alcohol, 2-methyl-5-ethylpyridine, 2-fluorine pyridine, five fluorine pyridines, 6-picoline-3-alcohol, pyridine-2-vinyl acetic monomer etc.
As pyrazole compound, can give an example as, pyrazoles, 1-allyl group-3,5-dimethyl pyrazole, 3,5-two (2-pyridyl) pyrazoles, 3,5-di-isopropyl pyrazoles, 3,5-dimethyl-1-hydroxymethylpyrazolcompound, 3,5-dimethyl-1-phenylpyrazole, 3，5-dimethylpyrazole, 3-amino-5-hydroxypyrazoles, 4-methylpyrazole, N-methylpyrazole, 3-amino-pyrazol, 3-amino-pyrazol etc.
As pyrimidine compound, can enumerate as, pyrimidine, 1,3-phenylbenzene-pyrimidine-2,4,6-triketone, Isosorbide-5-Nitrae, 5,6-tetrahydropyrimidine, 2,4,5,6-tetraminopyrimidine vitriol, 2,4,5-trihydroxy-pyrimidine, 2,4,6-Triaminopyrimidine, 2,4,6-trichloropyrimidine, 2,4,6-trimethoxy-pyrimidine, 2,4,6-triphenyl pyrimidine, 2,4-diamino-6-hydroxy pyrimidine, 2,4-di-amino-pyrimidine, 2-ethanamide pyrimidine, 2-aminopyrimidine, 4-amino-pyrazol be [3,4-d] pyrimidine etc. also.
As imidazolium compounds, can give an example as, 1,1'-carbonyl diurethane (1H-imidazoles), 1,1'-oxalyl diimidazole, 1,2,4,5-tetramethyl-imidazoles, 1,2-dimethyl-5-nitroimidazole, 1,2 dimethylimidazole, 1-(3-aminopropyl) imidazoles, 1-butyl imidazole, 1-ethyl imidazol(e), 1-Methylimidazole, benzoglyoxaline etc.
As guanidine compound, can give an example as, 1,1,3,3-tetramethyl guanidine, 1,2,3-triphenyl guanidine, 1,3-two-o-tolyl guanidine, 1,3-diphenylguanidine etc.
As thiazolium compounds, can give an example such as 2-mercaptobenzothiazole, 2 4-dimethylthiazole etc.
As tetrazole compound, can give an example as, tetrazolium, 5-methyl tetrazolium, 5-amino-1H-TETRAZOLE, 1-(2-dimethyl aminoethyl)-5-mercapto-tetrazole etc.
As triaizine compounds, can give an example as, 3,4-dihydro-3-hydroxy-4-oxo-1,2,4-triazine etc.
Above-mentioned corrosion inhibitor for metal can be used alone or mix two or more uses.The content of above-mentioned corrosion inhibitor for metal from obtaining the angle consideration for the good grinding rate that is polished film that contains cobalt element, preferably is 0.001 quality % ~ 10 quality % in the total mass of abrasive.Based on same viewpoint, the content of above-mentioned corrosion inhibitor for metal is more preferably more than the 0.01 quality %, further more than the preferred 0.02 quality %.In addition, based on same viewpoint, below preferred 5.0 % by weight of the content of above-mentioned corrosion inhibitor for metal, more preferably 0.5 % by weight.
Above-mentioned corrosion inhibitor for metal by combined with above-mentioned carboxylic acid derivative, even the etching speed that (for example, 50 ℃) also can significantly suppress the cobalt layer under harsh temperature condition grinds the cobalt layer with suitable speed simultaneously, can suppress the corrosion of cobalt layer.Think that this is that because for example under corrosion inhibitor for metal and above-mentioned specific dicarboxylic acid compound coexistence, performance is as excellent complex compound forming agent and the protectant function of film.
From the viewpoint, in the above-mentioned corrosion inhibitor for metal, be preferably and be selected from triazole compounds, pyridine compounds, imidazolium compounds, tetrazole compound, in triaizine compounds and the vulkacit H at least a kind, more preferably be selected from 3H-1,2,3-triazolo [4,5-b] pyridine-3-alcohol, I-hydroxybenzotriazole, 1H-1,2,3-triazolo [4,5-b] pyridine, the triazole compounds of benzotriazole etc., the 3-pyridone, benzoglyoxaline, 5-amino-1H-TETRAZOLE, 3,4-dihydro-3-hydroxy-4-oxo-1, at least a in 2,4-triazine and the vulkacit H.
Consider from the viewpoint of controlling well etching speed and grinding rate, the ratio of carboxylic acid derivative and corrosion inhibitor for metal (carboxylic acid derivative/corrosion inhibitor for metal) in the above-mentioned abrasive, preferred mass compares the scope 10/1 ~ 1/5, more preferably in 7/1 ~ 1/5 scope, further preferred 5/1 ~ 1/5 scope, the scope particularly preferably in 5/1 ~ 1/1.
Consider from the viewpoint of controlling well etching speed and grinding rate, further, in the above-mentioned abrasive, carboxylic acid derivative is preferably 10/1 ~ 1/5 with the ratio (carboxylic acid derivative/anticolodal) that is selected from least a corrosion inhibitor for metal in triazole compounds, pyridine compounds, imidazolium compounds, tetrazole compound, triaizine compounds and the vulkacit H
The ratio (carboxylic acid derivative/anticolodal) of at least a corrosion inhibitor for metal in above-mentioned carboxylic acid derivative and triazole compounds, pyridine compounds, imidazolium compounds, tetrazole compound, triaizine compounds and the vulkacit H more preferably 5/1 ~ 1/5
Above-mentioned carboxylic acid derivative, be selected from 3H-1,2,3-triazolo [4,5-b] pyridine-3-alcohol, I-hydroxybenzotriazole, 1H-1,2,3-triazolo [4,5-b] triazole compounds of pyridine, benzotriazole etc., and be selected from 3-pyridone, benzoglyoxaline, 5-amino-1H-TETRAZOLE, 3,4-dihydro-3-hydroxy-4-oxo-1, the ratio (carboxylic acid derivative/corrosion inhibitor for metal) of at least a kind corrosion inhibitor for metal in 2,4-triazine and the vulkacit H further preferred 5/1 ~ 1/1.
＜oxygenant＞
Above-mentioned abrasive preferably further contains at least a kind of oxygenant.Can by further containing oxygenant, more improve the grinding rate of cobalt layer layer in addition.Above-mentioned oxygenant has no particular limits, can be from normally used oxygenant appropriate selection.Particularly, such as hydrogen peroxide, sulfuric peroxide hydrochlorate, nitric acid, Potassium periodate, hypochlorous acid, ozone water etc., preferred hydrogen peroxide wherein.These metal onidiges can be used alone or mix two or more uses.
When abrasive contained oxygenant, the content of metal onidiges was preferably 0.01 quality % ~ 50 quality % in the total mass of abrasive.The viewpoint insufficient from the oxidation that prevents metal, that grinding rate descends is more than the preferred 0.02 quality % of described content, further more than the preferred 0.05 quality %.In addition, from preventing the face that is polished coarse angle consideration appears, below the preferred 30 quality %, further below the preferred 15 quality %.
＜organic solvent＞
In the above-mentioned abrasive, can also further contain organic solvent.By adding organic solvent, can improve the wettability that is arranged near the cobalt layer of cobalt layer layer in addition, can more improve grinding rate.As above-mentioned organic solvent, be not particularly limited preferred water miscible material.Water miscible definition herein is for 100g water, to dissolve the material more than the 0.1g in 25 ℃.
As above-mentioned organic solvent, can give an example as, the carbonate solvent of ethylene carbonate, Texacar PC, methylcarbonate, diethyl carbonate, Methyl ethyl carbonate etc.; The interior ester solvent of butyrolactone, propiolactone etc.; The diol solvent of ethylene glycol, propylene glycol, Diethylene Glycol, dipropylene glycol alcohol, triethylene glycol, tripropylene glycol etc.; The ether solvents of tetrahydrofuran (THF), diox, glycol dimethyl ether, polyethylene oxide, ethylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether acetic ester, propylene glycol methyl ether acetate etc.; The alcoholic solvent of methyl alcohol, ethanol, propyl alcohol, propyl carbinol, Pentyl alcohol, n-hexyl alcohol, Virahol, MMB etc.; The ketone solvent of acetone, methyl ethyl ketone etc.; Other organic solvents of dimethyl formamide, N-Methyl pyrrolidone, vinyl acetic monomer, ethyl lactate, tetramethylene sulfone etc. etc.
In addition, organic solvent also can be the derivative of diol solvent.Can enumerate such as, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, diethylene glycol monomethyl ether, diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, Tripropylene glycol monomethyl Ether, ethylene glycol monoethyl ether, dihydroxypropane single-ether, diethylene glycol monoethyl ether, DPE, Triethylene glycol ethyl ether, tripropylene glycol list ether, ethylene glycol ether, propylene glycol monopropyl ether, Diethylene glycol monopropyl ether, Triethylene glycol Monoisopropyl Ether, Tripropylene glycol Propyl Ether, ethylene glycol monobutyl ether, propylene glycol monobutyl ether, diethylene glycol monobutyl ether, Tri(propylene glycol)butyl ether,mixture of isomers, triethylene glycol butyl ether, the glycol monoether solvent of Tri(propylene glycol)butyl ether,mixture of isomers etc.; Glycol dimethyl ether, Propylene Glycol Dimethyl Ether, diethylene glycol dimethyl ether, the dipropylene glycol dme, triethylene glycol dimethyl ethyl ether, the tripropylene glycol dme, ethylene glycol diethyl ether, the propylene glycol diethyl ether, diethylene glycol diethyl ether, the dipropylene glycol diethyl ether, the triethylene glycol diethyl ether, the tripropylene glycol diethyl ether, the ethylene glycol bisthioglycolate propyl ether, the propylene glycol dipropyl ether, the Diethylene Glycol dipropyl ether, the dipropylene glycol dipropyl ether, the triethylene glycol dipropyl ether, the tripropylene glycol dipropyl ether, ethylene glycol dibutyl ether, the propylene glycol dibutyl ether, dibutyl ethylene glycol ether, the dipropylene glycol dibutyl ether, the triethylene glycol dibutyl ether, the glycol ether solvent of tripropylene glycol dibutyl ether etc. etc.
Wherein, organic solvent is preferably at least a in derivative, alcoholic solvent and the carbonate solvent that is selected from diol solvent, diol solvent, more preferably at least a in the alcoholic solvent.These organic solvents can be used alone or mix two or more uses.
When abrasive contained organic solvent, the content of organic solvent was preferably 0.1 quality % ~ 95 quality % in the total mass of abrasive.Consider from the angle that the wettability that prevents for the substrate of abrasive reduces, the content of above-mentioned organic solvent is more preferably more than the 0.2 quality %, further more than the preferred 0.5 quality %.In addition, become from the preparation that makes abrasive, use, wastewater treatment etc. and to be easy to angle and to consider, more preferably below the 50 quality %, further below the preferred 10 quality %.
＜water-soluble polymers＞
Above-mentioned abrasive preferably contains at least a kind of water-soluble polymers.More effectively reach thus the inhibition of corrosive effect, the protection on film surface, the minimizing that defective occurs etc.Herein, water miscible definition is, under 25 ℃, for the material more than the 100g water dissolution 0.1g.
As above-mentioned water-soluble polymers, can enumerate, have the water-soluble polymers of carboxylic acid group or carboxylate group etc.As such water-soluble polymers, can enumerate the autopolymer of the monomer with carboxylic acid group of vinylformic acid, methacrylic acid, toxilic acid etc.; The carboxylic acid group of this polymkeric substance becomes autopolymer that the carboxylate group of ammonium salt etc. forms etc.In addition, the monomer and the multipolymer with derivative of the monomer of carboxylate group and the alkyl ester of carboxylic acid etc. that also preferably have the carboxylic acid group.Can enumerate particularly such as, polymkeric substance that at least a portion of polyacrylic acid, polyacrylic carboxylic acid group is replaced by carboxylic acid ammonium's alkali (below, be called " ammonium polyacrylate salt ") etc. as water-soluble polymers.
In addition, as other water-soluble polymerss beyond above-mentioned, can give an example such as, the polyose of alginic acid, pectic acid, carboxymethyl cellulose, agar, curdlan, pulullan polysaccharide etc.; Polycarboxylic acid and the salt thereof of poly aspartic acid, polyglutamic acid, polylysine, polymalic acid, polyamic acid, polyamic acid ammonium salt, polyamic acid sodium salt, metaldehyde acid etc.; The vinyl based polymer of polyvinyl alcohol, polyvinylpyrrolidone, polyacrolein etc. etc.
When the substrate that grinds object is semiconductor integrated circuit with substrate etc., consider from the viewpoint of avoiding the pollution that above-mentioned basic metal, alkaline-earth metal, halogenide etc. cause, above-mentioned water-soluble polymers preferably has the polymkeric substance of acidic groups or their ammonium salt.But, when the substrate that grinds object is glass substrate etc., do not have such restriction.
In the above-mentioned water-soluble polymers, be preferably selected from the group of water-soluble polymers, pectic acid, agar, polymalic acid, polyacrylamide, polyvinyl alcohol and polyvinylpyrrolidone composition with carboxylic acid group or carboxylate group (when forming and obtaining ester, salt, comprise these) in water-soluble polymers, the water-soluble polymers (comprising ester, salt) that more preferably has carboxylic acid group or carboxylate group, further optimization polypropylene acid (comprising salt), particularly preferably ammonium polyacrylate salt.These can be used alone or mix two or more uses.
The weight-average molecular weight of water-soluble polymers is preferred 500 ~ 1,000,000, and more preferably 1,000 ~ 500,000, further preferred 2,000 ~ 200,000, particularly preferably 5,000 ~ 150,000.
Above-mentioned weight-average molecular weight for example can be measured by gel permeation chromatography (GPC) based on following method, can use the value that is converted into standard polypropylene acid to measure.
(condition)
Sample: 10 μ L
Standard polypropylene acid: Hitachi changes into テ Network ノ サ ー PVC ス Co., Ltd. trade(brand)name processed: PMAA-32
Detector: Hitachi Co., Ltd's system, RI-detector, trade(brand)name " L-3000 "
Integrator (integrator): Hitachi Co., Ltd's system, GPC-totalizing instrument, trade(brand)name " D-2200 "
Pump: Hitachi Co., Ltd's system, trade(brand)name " L-6000 "
De-gassing vessel: Showa Denko K. K's system, trade(brand)name " Shodex DEGAS "
Chromatographic column: Hitachi Chemical Co., Ltd.'s system, with the use that is linked in sequence of trade(brand)name " GL-R440 ", " GL-R430 ", " GL-R420 "
Elutriant: tetrahydrofuran (THF) (THF)
Measure temperature: 23 ℃
Flow velocity: 1.75mL/ minute
Minute: 45 minutes
During abrasive containing water-soluble polymkeric substance, the preferred 0.001 quality % of the content of water-soluble polymers in the total mass of abrasive ~ 10 quality %.Consider from the viewpoint that can guarantee good corrosion-inhibiting, more than the preferred 0.001 quality %, more preferably more than the 0.01 quality %, further more than the preferred 0.02 quality %.In addition, consider from the angle that can keep sufficient grinding rate, below the preferred 10 quality %, more preferably below the 5.0 quality %, further below the preferred 1.0 quality %.
＜abrasive particle＞
Above-mentioned abrasive preferably contains at least a kind of abrasive particle.By containing abrasive particle, can improve the grinding rate that is arranged near the cobalt layer of cobalt layer layer in addition.
As main abrasive particle, can give an example as, the organism polishing particles of the inorganics polishing particles of silicon-dioxide, aluminum oxide, zirconium white, cerium dioxide, titanium dioxide, germanium oxide, silicon carbide etc., polystyrene, polyacrylic acid, polyvinyl chloride etc. etc.This wherein is preferably selected from the inorganics polishing particles of silicon-dioxide, aluminum oxide, zirconium white, cerium dioxide, titanium dioxide and germanium oxide, especially, more preferably is selected from the inorganics polishing particles of silicon-dioxide and aluminum oxide.
The grinding good, that produced by CMP of dispersion stabilization from abrasive damages (scratch, scratch) angle that generation quantity is few is considered, by preferred colloid silica or colloidal alumina, more preferably colloid silica in the inorganics polishing particles of selecting in silicon-dioxide and the aluminum oxide.These abrasive particles can be used alone or mix two or more uses.
Consider from the angle that can obtain good grinding rate, the median size of abrasive particle is preferably at 10nm ~ 100nm, more preferably at 20nm ~ 90nm, further preferably at 40nm ~ 80nm.
The median size of abrasive particle is with light diffraction scattering formula size-grade distribution meter (for example, the trade(brand)name of COULTER ELectronics society system: the value of COULTER N4SD) measuring.The condition determination of Coulter is, measure 20 ℃ of temperature, solvent specific refractory power 1.333(and water when), particle specific refractory power Unknown(sets), solvent viscosity 1.005MPaS(and water ought), 90 ° of Run Time 200sec, laser input angle, make Intensity(be equivalent to scattering strength, turbidity) in the scope of 5E+04 ~ 4E+05, when being higher than 4E+05, measure behind the dilute with water.
When abrasive contained abrasive particle, the content of abrasive particle was preferably in the total mass of abrasive more than the 1.0 quality %, more preferably more than the 3.0 quality %, and further preferred 3.0 quality % ~ 5.0 quality %.Be set in above-mentioned scope by the content with above-mentioned abrasive particle, can obtain good grinding rate.
＜water＞
There is no particular limitation for the water that the present invention uses, and can preferably use pure water.Water is so long as mixed as the remainder of the constituent material of above-mentioned abrasive, and content has no particular limits.
＜other 〉
Can make an addition to other compositions in the above-mentioned abrasive, for example as, the tinting material of the pigment of the dyestuff of tensio-active agent, Victoria pure blue etc., phthalocyanine green etc. etc.
The pH of above-mentioned abrasive is below 4.0.If pH surpasses 4.0, the conductive material layer that is then formed with metal by wiring and the grinding rate of cobalt layer may descend.On the other hand, from suppressing to corrode at leisure wiring with metal in addition, because the strong and reluctant angle of acidity is set out, above-mentioned pH is preferably more than 1.0, more preferably more than 2.0.
PH can adjust by the addition of acidic cpd.In addition, also can adjust by the interpolation of the basic cpds such as ammonia, sodium hydroxide, Tetramethylammonium hydroxide (TMAH).
(for example, the Model F-51 of Horiba Ltd (HORIBA, Ltd.) system measures the mensuration of the pH of above-mentioned abrasive with pH meter.Can Application standard damping fluid (phthalate pH pH of buffer: 4.21(25 ℃), neutral phosphonic hydrochlorate pH pH of buffer: 6.86(25 ℃), borate pH pH of buffer: 9.04(25 ℃)) carry out 3 point calibrations after, electrode is inserted in the abrasive, measure through the value after stable more than 3 minutes.
Above-mentioned abrasive can be used as abrasive (stock solution) keeping that contains carboxylic acid derivative, corrosion inhibitor for metal and water, during grinding, this abrasive, other constituent materials and water is suitably mixed use.Perhaps, also can and use with the state keeping of the abrasive that suitably mixes other constituent materials in carboxylic acid derivative, corrosion inhibitor for metal and the water.
Above-mentioned abrasive is applicable to the formation of the wiring layer in the semiconducter device.The film that is polished as grinding object as long as contain the part (hereinafter referred to as " cobalt part ") that contains at least cobalt element, further, also can contain near the conductive material, barrier metal or the isolator that are arranged at cobalt section.
Namely, other forms of the present invention, being abrasive contains purposes in the layer of cobalt element in grinding, described abrasive contains by being selected from phthalic compounds, m-phthalic acid compound and the alkyl dicarboxylic carboxylic acid cpd of following general formula (I) expression and carboxylic acid derivative, corrosion inhibitor for metal and the water of at least a formation in their salt and the acid anhydrides, and pH is below 4.0.
HOOC-R-COOH…(I)
(in the above-mentioned general formula (I), R represents that carbonatoms is 4 ~ 10 alkylidene group.）
In addition, other forms of the present invention are, abrasive grinding contain cobalt element the layer in purposes, described abrasive contains and is selected from phthalic compounds, m-phthalic acid compound and alkyl dicarboxylic aid's compound of following general formula (I) expression and at least a carboxylic acid derivative, corrosion inhibitor for metal and the water in their salt and the acid anhydrides, pH is below 4.0, in the time of 50 ℃, for the etching speed of cobalt below 10.0nm/min.
HOOC-R-COOH…(I)
(in the above-mentioned general formula (I), R represents that carbonatoms is 4 ~ 10 alkylidene group.）
[substrate Ginding process]
Substrate Ginding process of the present invention is, uses upper film that is polished that contains cobalt element that forms at least one surface of above-mentioned abrasive grinding base plate, removes the Ginding process of the unnecessary part that contains cobalt element.More specifically, what form at least one surface of substrate contains being polished between the abrasive cloth on film and the grinding plate of cobalt element, supply with above-mentioned abrasive, to be provided with simultaneously the above-mentioned described substrate surface that is polished the face side of film is pressed under the state of abrasive cloth, by this substrate and grinding plate are relatively moved, remove the Ginding process of at least a portion that is polished film.
Below, the series of processes of using wiring layer substrate Ginding process of the present invention, in the semiconducter device to form is described with reference to Fig. 2.But the purposes of abrasive of the present invention is not limited to following operation.
Shown in Fig. 2 (a), substrate 10 before grinding, have at silicon substrate 1: the barrier metal layer 3 and the cobalt layer 4 that covers barrier metal layer 3 of the isolator 2 that the isolator 2 of the recess of predetermined pattern is arranged, covers along the convex-concave on the surface of this isolator 2 are formed with conductive material layer 5 at cobalt layer 4.
There can be exemplified that as isolator 2 silicon is isolator, organic polymer system isolator etc.Be isolator as silicon, can enumerate, the silica-based isolator of the organic silicate glass that obtains as starting raw material take silicon-dioxide, fluorosilicate glass, trimethyl silane or dimethoxy dimethylsilane, silicon oxynitride, hydrogen silsesquioxanes etc. or, silicon carbide and silicon nitride etc.In addition, as organic polymer system isolator, can enumerate all aromatic is low dielectric constant insulator.Wherein, especially preferred silicon-dioxide.
Isolator 2 is by the CVD(chemical gaseous phase deposition) method, spin-coating method, dip coating or spraying method film forming.As the object lesson of isolator 2, can enumerate such as LSI manufacturing process, particularly multilayer wiring and form isolator in the operation etc.
Barrier metal layer 3 forms for the adaptation that prevents conductive material and be diffused in the isolator 2 and improve between isolator 2 and the conductive material layer 5.As the barrier metal that is used for barrier metal layer 3, the tantalum compound of tantalum, tantalum nitride, tantalum alloy etc. is arranged for example, the titanium compound of titanium, titanium nitride, titanium alloy etc., the tungsten compound of tungsten, tungsten nitride, tungstenalloy etc., the ruthenium compound of ruthenium etc. etc.Barrier metal layer 3 can be by a kind of single layer structure that forms in these, also can be the lamination structure of two or more formation.Barrier metal layer 3 is by evaporation, CVD(chemical gaseous phase deposition) etc. film forming.In addition, as barrier metal layer 3 cobalt layer 4 can only be set.
As the cobalt class that adopts in the cobalt layer 4, can enumerate the oxide compound of cobalt, cobalt-base alloy, cobalt, the oxide compound of cobalt-base alloy etc.The cobalt layer is by film forming such as known gunitees.
As the conductive material that adopts in the conductive material 5, can enumerate the metal take copper as main component of the oxide compound of copper, copper alloy, copper, the oxide compound of copper alloy etc., the tungsten metal of tungsten, tungstenalloy etc., the precious metal such as silver-colored, golden etc.The metal take copper as principal constituent of oxide compound of the oxide compound of preferably copper, copper alloy, copper, copper alloy etc. wherein.Conductive material layer 5 is by film forming such as known gunite, electrochemical plating.
The thickness of preferred isolator 2 is about 0.01 μ m ~ 2.0 μ m, and the thickness of barrier metal layer 3 is about 0.01 μ m ~ 2.5 μ m, and the thickness of cobalt layer 4 is at 0.01 μ m ~ 2.5 μ m, and the thickness of conductive material layer 5 is about 0.01 μ m ~ 2.5 μ m.
Be ground to the 1st grinding step of the conductive material layer 5 of state shown in Fig. 2 (b) from state shown in Fig. 2 (a), example as, the abrasive that the grinding rate of conductive material layer 5/ cobalt layer 4 is used than enough large conductive material, the conductive material layer 5 that will grind the surface of front substrate 10 by CMP grinds.Thereby the cobalt layer 4 that obtains the protuberance on the substrate is exposed to the residual substrate with conductive pattern 20 that conductive material layer 5 is arranged in surface, the recess.As the abrasive that the grinding rate of conductive material layer 5/ cobalt layer 4 is used than enough large above-mentioned conductive material, the abrasive of putting down in writing in energy example such as No. 3337464 specification sheets of Japanese Patent.Also can grind the part that conductive material layer 5 grinds the cobalt layer 4 of protuberance together in the 1st grinding step.
In ensuing the 2nd grinding step, the conductive pattern that will obtain by the 1st grinding step is polished film as what the 2nd grinding step was used, uses abrasive of the present invention to grind.
In the 2nd grinding step, press at the abrasive cloth of grinding plate under the state of substrate 20, between abrasive cloth and substrate, supply with abrasive of the present invention, by making grinding plate and substrate 20 relatively mobile, grind the cobalt layer 4 by exposing in the 1st grinding step simultaneously.
As milling apparatus, can use general milling apparatus, have the upholder that keeps polished substrate in its device, be connected and pasted the grinding plate of abrasive cloth with the motor of variable rotating speed etc.As abrasive cloth, can use common non-woven fabrics, urethane foam, Porous fluoro-resin etc., have no particular limits.
Grinding condition has no particular limits, but the following low rotation of the preferred 200rpm of the speed of rotation of grinding plate.So that substrate does not fly out.Press the pressure with the substrate that is polished film on the abrasive cloth, preferred 1kPa ~ 100kPa is polished the homogeneity of the grinding rate in the face and the flatness of pattern, more preferably 5kPa ~ 50kPa in order to satisfy.
In the grinding, use continuously pump etc. to abrasive cloth be polished supply abrasive of the present invention between the film.This feed rate has no particular limits, but the total surface of preferred abrasive cloth is to be polished agent to cover.Substrate after grind finishing makes it dry after preferably carefully brushing lightly the water droplet that falls to being attached on the substrate with Rotary drying etc. after the washing in flowing water.
In the 2nd grinding step, grind at least the cobalt layer 4 that exposes, remove unnecessary cobalt part.In the 2nd grinding step, grind cobalt layer 4, just finish to grind if expose barrier metal layer 3, also can use in addition the abradant abrasive of barrier metal layer to grind barrier metal layer 3.In addition, as from Fig. 2 (b) to shown in Fig. 2 (c), also can be ground to metal level 3 from cobalt layer 4 in the 2nd grinding step a series ofly.Further, the conductive layer 5 that is embedded in recess can be polished with cobalt layer 4 and barrier metal layer 3.
In the moment of the substrate 30 that obtains having desirable pattern, finish to grind, desirable pattern is as follows, isolator 2 under the barrier metal layer 3 of protuberance all exposes, in the recess residual have become the conductive material of wiring layer layer 5, expose in the cross section of barrier metal layer 3 and cobalt layer 4 in the border between protuberance and the recess.
More excellent flatness when finishing in order to ensure grinding, further, as shown in Figure 3, over-mastication (for example, time till the 2nd grinding step obtains desirable pattern is when being 100 seconds, except this grinding of 100 seconds, append again and ground in 50 seconds, be called over-mastication 50%) also passable.During over-mastication, the part of isolator 2 also is removed because of grinding.
On the metal line that forms like this, further form the 2nd layer isolator and metal line after, grind, make whole faces of semiconductor substrate become level and smooth face.Repeat this operation by stipulated number, can make the semiconducter device with desirable wiring number of plies.
Abrasive of the present invention is not only the grinding of the metallic membrane that forms in the semiconductor substrate described above, also can be used for the substrate of lapping magnetic heads etc.
[embodiment]
Below, by embodiment the present invention is carried out more specific description, but the present invention is not limited by these embodiment.
＜for the evaluation of the etch quantity of cobalt＞
［ embodiment and comparative example ］
(making method of abrasive)
Join respectively the corrosion inhibitor for metal shown in table 1 and the table 2 and carboxylic acid derivative in the container, so that become the combined amount of putting down in writing as in the table 1 as the amount of final abrasive, and (Hitachi changes into テ Network ノ サ ー PVC ス system to add the ammonium polyacrylate salt that makes as water-soluble polymers, molecular weight 8000) becomes the amount of 0.02 quality % of final abrasive, making MMB as organic solvent is the amount of 1.4 quality % of final abrasive, to wherein injecting ultrapure water, mix, dissolve whole compositions.
Then, add 4.0 quality % in the total mass of the slurries be equivalent to prepare amount, as the colloid silica (Fukawa Chemical Industries Co., Ltd.'s system, particle diameter 60nm) of the silicon dioxide granule of abrasive particle, re-inject ultrapure water, obtain slurries.In the total mass of the slurries that obtain, the hydrogen peroxide that adds 30 quality % is 0.2 quality %, obtains various abrasives.
The pH of each abrasive that mensuration obtains the results are shown in Table 1 and table 2.
(estimating the etch quantity for cobalt)
It is the shell substrate (a) of the cobalt layer of 300nm that preparation has formed thickness at 8 inches silicon substrate with the CVD method.Above-mentioned shell substrate (a) is cut into the square chip of 20mm, prepares to estimate with chip (b).
In the beaker of each abrasive 50g of above-mentioned adding, add respectively above-mentioned evaluation with chip (b), in 50 ℃ thermostatic bath, soaked 1 minute.Take out the chip (b) after soaking, after fully washing with pure water, spray nitrogen makes the moisture drying on the chip.Dried evaluation is fixed with the resistivity instrumentation with the resistance of chip (b), is converted into the thickness of the cobalt layer after the immersion in the following formula (1).
From obtaining lubber-line the information of corresponding resistance value respectively with each thickness of shell basic unit (a), try to achieve the thickness of cobalt layer by following formula (1).
The thickness [nm] of the cobalt layer after the immersion
=104.5 * (estimating the resistance value [m Ω]/1000 with chip (b)) -0.893
Then, the thickness of the cobalt layer after the immersion that obtains with soak before the thickness of cobalt layer, according to following formula (2), try to achieve the etching speed of cobalt layer.
The etching speed of cobalt layer (Co-ER) [nm/min]
=(thickness [nm] of the cobalt layer after the thickness [nm] of the cobalt layer before soaking-immersion)/1 minute ... (2)
To each abrasive obtained above, try to achieve the etching speed for the cobalt layer.This results are shown in Table 1 and table 2.In addition, in table 1 and the table 2, "-" expression in the hurdle of carboxylic acid derivative and anticolodal is unmixed.
(for the evaluation of the grinding rate of cobalt layer)
Grinding rate (Co-RR) [nm/min] when in addition, evaluation uses each abrasive obtained above to grind under the following conditions above-mentioned shell substrate (a).This result is shown in table 1 and the table 2 in the lump.In addition, about several comparative examples, because etching speed is too fast, the evaluation of therefore omitting grinding rate is recited as "-".
＜grinding condition＞
Abrasive cloth: IC1000
Grinding pressure: 10.3kPa(1.5psi)
Rotating speed: platform/grinding head=93/87rpm
The feed rate of abrasive: 200mL/ minute
Milling time: 0.5 minute
[table 1]
[table 2]
Figure BDA00001912864900201
Very clear from table 1 and table 2, among the embodiment 1 ~ 13, by containing simultaneously specific dicarboxylic acid and corrosion inhibitor for metal, even under 50 ℃ condition, also significantly suppress the etching speed of cobalt, can grind the cobalt layer with suitable speed as can be known.Thus, enlightenment: in containing the abrasive of the present invention of above-mentioned carboxylic acid derivative, above-mentioned specific dicarboxylic acid compound has the effect as complex compound forming agent and inhibitor concurrently.That is, according to abrasive of the present invention, enlightenment contains when layer of cobalt element in grinding, and by over etching, or because corrosion produces slit with good grinding rate grinds and establishment contains cobalt element layer.

Claims (8)

1. abrasive, be used for grinding the layer that contains cobalt element, described abrasive contains and is selected from by phthalic compounds, m-phthalic acid compound and the alkyl dicarboxylic carboxylic acid cpd of following general formula (I) expression and carboxylic acid derivative, corrosion inhibitor for metal and the water of at least a formation in their salt and the acid anhydrides, the pH of abrasive is below 4.0
HOOC-R-COOH…(I)
In the above-mentioned general formula (I), R represents that carbonatoms is 4 ~ 10 alkylidene group.
2. abrasive, be used for grinding the layer that contains cobalt element, described abrasive contains and is selected from phthalic compounds, m-phthalic acid compound and alkyl dicarboxylic aid's compound of following general formula (I) expression and at least a carboxylic acid derivative, corrosion inhibitor for metal and the water in their salt and the acid anhydrides, the pH of abrasive is below 4.0, in 50 ℃, abrasive for the etching speed of cobalt below 10.0nm/min
HOOC-R-COOH…(I)
In the above-mentioned general formula (I), R represents that carbonatoms is 4 ~ 10 alkylidene group.
3. such as claim 1 or abrasive claimed in claim 2, described corrosion inhibitor for metal contains the compound with triazole skeleton.
4. such as the described abrasive of any one in claim 1 ~ claim 3, further contain oxygenant.
5. such as the described abrasive of any one in claim 1 ~ claim 4, further contain organic solvent.
6. such as the described abrasive of any one in claim 1 ~ claim 5, further contain water-soluble polymers.
7. such as the described abrasive of any one in claim 1～claim 6, further contain abrasive particle.
8. substrate Ginding process, right to use require the described abrasive of any one in the 1～claim 7 to grind the film that is polished that contains cobalt element that forms at least one surface of substrate, remove the redundance that contains cobalt element.
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