CN1170909C - Chemical mechanical plane of metal wiring - Google Patents
Chemical mechanical plane of metal wiring Download PDFInfo
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- CN1170909C CN1170909C CNB99121580XA CN99121580A CN1170909C CN 1170909 C CN1170909 C CN 1170909C CN B99121580X A CNB99121580X A CN B99121580XA CN 99121580 A CN99121580 A CN 99121580A CN 1170909 C CN1170909 C CN 1170909C
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Abstract
The present invention relates to a chemical and mechanical plane process for removing copper or copper alloy in ground sherry. The ground sherry comprises corrosive agent, oxidizing inhibitor and additive, wherein the additive obviously regulates the match between copper and oxidizing inhibitor.
Description
The present invention relates generally to the unicircuit metallization, particularly relate to the method for planarizing of copper wiring.
In the field that unicircuit is made, people are perfectly clear and form the advantage (' metallization pattern ' couples together one or more transistors, electric capacity, resistance and other the electronic devices and components on the wafer that are formed on) of the great integration density aspect that planar metallised figure brought here.In industry, important tendency is to use so-called ' grinding and polishing that obtains with the chemical-mechanical mode ' (or ' CMP polishing ', or ' CMP ') technology to produce so planar metallised figure.In CMP, front one side of wafer is retained as towards the grinding and polishing wheel that rotates, and imports a kind of chemical grout simultaneously, and the combination by chemical reaction and physical abrasion makes one or more metal levels of wafer top be removed.For example, authorize people's such as Beyer No. 4944836, patent US referring to July 31 nineteen ninety, it has transferred transferee of the present invention (the CMP method of the metal flatization of passivation relatively, or the CMP method of the passivation complanation of metal line) relatively.
Remove with outside the CMP resulting general advantage the special advantage aspect the density that the integrated metal wiring that forms can bring in the complanation in advance of passivation.Just as indicated in authorizing people such as Chow on December 6th, 1998 and transferring among the transferee's of the present invention patent US 4789648 (being referred to as ' ChowShi patent ' from now on), (this is a single metal layer in the integrated metal wiring, comprise a vertical part, this part extends downwardly into the layer that is tiled in the wafer top so that contact with the electricity conductive construction that forms above that, the part that also comprises a level, this part provides a kind of electrical connection) forming process be first deposit and determine by making it the aperture of two passivation layers after the complanation with CMP, then at whole structure top depositing metal and grind away the part metals of the passivation layer top that extends to complanation.Usually, the level of metal line and vertical component form with double layer of metal.The ChowShi patent has obtained maximum electric conductivity by eliminate usually the way of the interface layer that exists between the level of metal line structure and vertical component.
In the prior art, well-known is to utilize aluminium alloy or tungsten as the metal line that uses for unicircuit.But along with minimized size on the sheet is reduced to below 0.25 micron, the conductive characteristic of these materials just no longer meets the demands.These metal lines are typically said so and are utilized chemical vapour deposition or other deposition technology to be deposited to the wafer top.Along with interconnect dimensions reduces, will increase by the transitional pore of interlayer dielectric formation or the aspect ratio (being depth-width ratio) of through hole, cause in utilizing the directional technology metals deposited, forming the space.In addition, in the littler metal line of geometrical dimension, will become more responsive to electromigration invalidation.Therefore, in nearest development, developed a kind of copper wiring technique.Copper has low resistivity, high deelectric transferred ability, and can utilize the electroplating technology of the formation that reduces the space widely to carry out deposit.But, because copper is a kind of soft metal that does not have height protectiveness native oxide, and can not be easily graphical with the reactive ion etching technology of standard, so particularly in the CMP field, it proposes a kind of unique challenges.
The various slurry of using for the CMP of copper (and/or for the copper use stop (barrier) material) have been carried in the prior art.These technology comprise following:
1) nitric acid, a kind of polymkeric substance, a kind of tensio-active agent and sulfuric acid or sulfonic acid in a kind of non-CMP technology, are used for removing copper (the patent US 4632727 of Nelson, this patent transfers Psi Star) from printed circuit board.
2) iron-ammonia-EDTA (USP 4954142, and people's such as Patrick patent also transfers transferee of the present invention).
3) water, solid-state abradant, and HNO
3, H
2SO
4And AgNO
3In one of (US 5225034 and division 5534490 are to authorize people's such as Yu and transfer the patent of Micron Technology)
4) a kind of oxygenant and a kind of silica abrasive, the slurry of PH between 2 and 4 are used for grinding and polishing tungsten, copper, titanium nitride, or tungsten silicide (US 5340370 and division 5516346, it be authorize Cadient etc. the people's and transfer the patent of Intel)
5) PH is ammonium persulphate/KOH (" copper being carried out the alkalescence prescription of cmp polishing with pyrroles (Azole) passivation ", IBM Technical Disclosure Bulletin, 37 volumes, the 10th phase, in October, 1994, the 187th page) of 10.
6) silicon-dioxide or alumina particulate, Padil, and hydrogen peroxide (european patent application 94119785.7,6/28/95 based on JP 313406/93 is published).
7) colloidal silica, Textone, deionized water (US 5451551, authorize people such as Krishnan September 5 nineteen ninety-five)
8) a kind of oxygenant, a kind of tensio-active agent and deionized water, has homodisperse aluminium oxide particles, this aluminium oxide particles has that (US 5527423 less than about 1 micron coacervate distribution of sizes with less than about 0.4 micron mean diameter, on June 8th, 1996 was authorized people such as Neville, and transferred Cabot Inc.).
9) iron nitrate, BTA, poly-(ethylene glycol) and aluminium oxide particles (" the copper CMP polishes in acidic medium ", people such as Luo, the 1996CMP-MIC meeting, February 22-23 1996, the 145-51 pages or leaves).
10) in the 1st CMP slurry, use aluminium oxide particles grinding and polishing bulk metal (tungsten or copper), in the 2nd CMP slurry, use the Ti/TiN (US5676587 of silicon dioxide granule grinding and polishing lower floor then, authorized people such as Landers on October 14th, 1997 and transfer transferee's of the present invention patent) and
11) silicon-dioxide, glycine, BTA (US 5770095, authorize people and the patent that transfers Toshiba Corp. such as Sasaki).
In general, cited prior art all relates to the polishing (in some cases, also relating to blocking material) of the copper in common metal line or keyhole application more than.But, when as during at ChowShi patent grinding and polishing metal, will face the special challenge that in CMP technology, must run into.
In the present invention, comprising oxygenant, oxidation retarder and obviously regulating in the slurry of oxidation retarder to the additive of the cooperation of copper, remove copper with CMP, the result can obtain high copper removal rate and can not remove the metal or the dielectric layer of lower floor significantly or cause tangible copper corrosion, and has the loss of minimum copper in graphical interconnection.
In a first aspect of the present invention, a kind of CMP slurry that is used for grinding and polishing copper layer or copper alloy layer is provided, comprise etching reagent, oxidation retarder and additive, this additive is regulated the cooperation between copper and the oxidation retarder significantly.
In a second aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: above-mentioned etching reagent is selected from: iron nitrate and compound thereof, hydrogen peroxide, Potassium Iodate, manganese oxide, ammonium hydroxide, ammonium persulphate, Potassium Persulphate, ammonium persulphate/sulfuric acid, Potassium Persulphate/sulfuric acid, iron(ic) chloride/hydrochloric acid, chromic acid, chromic acid/hydrochloric acid, potassium bichromate/sulfuric acid and iron stearate (III) salt.
In a third aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: above-mentioned etching reagent comprises iron nitrate.
In a fourth aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: above-mentioned oxidation retarder is selected from: the 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
In a fifth aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: above-mentioned oxidation retarder comprises BTA.
In a sixth aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: above-mentioned additive comprises the sodium salt of sulfated fatty alcohol.
In a seventh aspect of the present invention, a kind of slurry according to above-mentioned the 6th aspect is provided, it is characterized in that: above-mentioned sodium salt has the molecular weight less than about 350.
In a eighth aspect of the present invention, a kind of slurry according to above-mentioned the 6th aspect is provided, it is characterized in that: above-mentioned sodium salt does not form the micella that is higher than micelle-forming concentration.
In a ninth aspect of the present invention, a kind of slurry according to above-mentioned the 7th aspect is provided, it is characterized in that: the sodium salt of above-mentioned sulfated fatty alcohol is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, Duponol SP and Duponol WN.
In a tenth aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: above-mentioned additive comprises Duponol SP.
In a eleventh aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: also comprise colloidal alumina.
In a twelveth aspect of the present invention, a kind of slurry according to above-mentioned the tenth one side is provided, it is characterized in that: above-mentioned colloidal alumina has particle diameter less than about 0.3 micron particulate.
In a thirteenth aspect of the present invention, a kind of slurry according to above-mentioned first aspect is provided, it is characterized in that: above-mentioned slurry has the PH of 1.2-2.5.
In a fourteenth aspect of the present invention, a kind of CMP slurry of grinding and polishing at the copper layer or the copper alloy layer of lining top that be used for is provided, this slurry provides the 1st of above-mentioned copper or copper alloy to remove speed, remove speed with the 2nd of above-mentioned lining, the above-mentioned the 1st removes speed, and to remove speed than the above-mentioned the 2nd at least big 50 times, this slurry comprises etching reagent, oxidation retarder and additive, and this additive is regulated the cooperation between copper and the oxidation retarder significantly.
In a fifteenth aspect of the present invention, a kind of slurry according to above-mentioned the 14 aspect is provided, it is characterized in that: above-mentioned etching reagent is selected from: iron nitrate and compound thereof, hydrogen peroxide, Potassium Iodate, manganese oxide, ammonium hydroxide, ammonium persulphate, Potassium Persulphate, ammonium persulphate/sulfuric acid, Potassium Persulphate/sulfuric acid, iron(ic) chloride/hydrochloric acid, chromic acid, chromic acid/hydrochloric acid, potassium bichromate/sulfuric acid and iron stearate (III) salt.
In a sixteenth aspect of the present invention, a kind of slurry according to above-mentioned the 15 aspect is provided, it is characterized in that: above-mentioned etching reagent comprises iron nitrate.
In a seventeenth aspect of the present invention, a kind of slurry according to above-mentioned the 14 aspect is provided, it is characterized in that: above-mentioned oxidation retarder is selected from: the 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
In a eighteenth aspect of the present invention, a kind of slurry according to above-mentioned the 14 aspect is provided, it is characterized in that: above-mentioned oxidation retarder comprises BTA.
In a nineteenth aspect of the present invention, a kind of slurry according to above-mentioned the 14 aspect is provided, it is characterized in that: above-mentioned additive comprises the sodium salt of sulfated fatty alcohol.
In a twentieth aspect of the present invention, a kind of slurry according to above-mentioned the 19 aspect is provided, it is characterized in that: above-mentioned sodium salt has the molecular weight less than about 350.
In the 20 one side of the present invention, a kind of slurry according to above-mentioned the 20 aspect is provided, it is characterized in that: above-mentioned sodium salt does not form the micella that is higher than micelle-forming concentration.
Aspect the of the present invention the 22, provide a kind of according to the above-mentioned the 20 on the one hand slurry, it is characterized in that: the sodium salt of above-mentioned sulfated fatty alcohol is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, Duponol SP, Duponol WN.
Aspect the of the present invention the 23, a kind of slurry according to above-mentioned the 14 aspect is provided, it is characterized in that: above-mentioned additive comprises Duponol SP.
Aspect the of the present invention the 24, a kind of slurry according to above-mentioned the 14 aspect is provided, it is characterized in that: also comprise colloidal alumina.
Aspect the of the present invention the 25, a kind of slurry according to above-mentioned the 24 aspect is provided, it is characterized in that: above-mentioned colloidal alumina has particle diameter less than 0.3 micron particulate.
Aspect the of the present invention the 26, a kind of slurry according to above-mentioned the 14 aspect is provided, it is characterized in that: above-mentioned slurry has the PH for 1.2-2.5.
Aspect the of the present invention the 27, provide a kind of grinding and polishing that is used in the copper layer of lining top or the slurry of copper alloy layer, the low combination of removing speed that above-mentioned slurry provides the height of above-mentioned copper or copper alloy to remove speed and above-mentioned lining, and comprise acid attack agent, oxidation retarder, colloidal alumina and sulfated fatty alcohol tensio-active agent.
In the 20 eight aspect of the present invention, a kind of slurry according to above-mentioned the 27 aspect is provided, it is characterized in that: above-mentioned colloidal alumina accounts for the 0.3-3 weight % of above-mentioned slurry.
Aspect the of the present invention the 29, a kind of slurry according to above-mentioned the 27 aspect is provided, it is characterized in that: every liter above-mentioned slurry contains the above-mentioned acid attack agent of 2 grams at least.
Aspect the of the present invention the 30, a kind of slurry according to above-mentioned the 27 aspect is provided, it is characterized in that: every liter above-mentioned slurry contains 3 milliliters of above-mentioned tensio-active agents at least.
Aspect hentriaconta-of the present invention, provide a kind of and comprising that wafer carries the method for grinding and polishing copper in the CMP instrument of holding device and grinding and polishing dish or copper alloy, this method comprises the steps:
The wafer that has the copper layer on the surface thereon is placed into wafer to be carried and holds in the device;
The slurry that comprises etching reagent, oxidation retarder and sulfated fatty alcohol tensio-active agent is added on the above-mentioned grinding and polishing dish, and above-mentioned tensio-active agent has the molecular weight less than 350, and regulate significantly between copper and the above-mentioned oxidation retarder cooperation and
The above-mentioned wafer of way grinding and polishing that employing makes above-mentioned copper layer contact with above-mentioned grinding and polishing dish.
Aspect the of the present invention the 32, a kind of method according to above-mentioned hentriaconta-aspect is provided, it is characterized in that: above-mentioned slurry is added to above-mentioned steps on the above-mentioned grinding and polishing dish, is to finish before carrying the above-mentioned steps of holding on the device above-mentioned wafer being placed into above-mentioned wafer.
Aspect the of the present invention the 33, a kind of method according to above-mentioned hentriaconta-aspect is provided, it is characterized in that: above-mentioned etching reagent comprises iron nitrate.
Aspect the of the present invention the 34, a kind of method according to above-mentioned the 33 aspect is provided, it is characterized in that: above-mentioned oxidation retarder is selected from: the 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
Aspect the of the present invention the 35, a kind of method according to above-mentioned hentriaconta-aspect is provided, it is characterized in that: above-mentioned tensio-active agent comprises sulfation lipid acid.
Aspect the of the present invention the 36, a kind of method according to above-mentioned the 35 aspect is provided, it is characterized in that: above-mentioned sulfation lipid acid is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, Duponol SP and Duponol WN.
Aspect the of the present invention the 37, a kind of method according to above-mentioned hentriaconta-aspect is provided, it is characterized in that: above-mentioned slurry has the PH of 1.2-2.5.
In the 30 eight aspect of the present invention, a kind of method according to above-mentioned hentriaconta-aspect is provided, it is characterized in that: above-mentioned grinding and polishing dish comprises nonwoven grinding and polishing dish.
Aspect the of the present invention the 39, a kind of method according to above-mentioned the 30 eight aspect is provided, it is characterized in that: above-mentioned grinding and polishing step is carried out under the also low temperature of the temperature of being out of shape significantly than above-mentioned nonwoven grinding and polishing dish.
Aspect the of the present invention the 40, a kind of instrument that the copper on the blocking layer top that is configured in the workpiece top or copper alloy are carried out CMP of being used for is provided, it comprises:
A wafer that is used for keeping wafer carries and holds device;
One carries with wafer in CMP operating period and to hold the grinding and polishing dish that the wafer in the device contacts;
A kind of slurry, this slurry provides the 1st of above-mentioned copper or copper alloy to remove speed, remove speed with the 2nd of above-mentioned blocking layer, the above-mentioned the 1st removes speed, and to remove speed than the above-mentioned the 2nd at least big 50 times, this slurry comprises etching reagent, oxidation retarder and additive, and this additive is regulated the cooperation between copper and the oxidation retarder significantly.
The of the present invention the 40 on the one hand, a kind of instrument according to above-mentioned the 40 aspect is provided, it is characterized in that: above-mentioned etching reagent is selected from: iron nitrate and compound thereof, hydrogen peroxide, Potassium Iodate, manganese oxide, ammonium hydroxide, ammonium persulphate, Potassium Persulphate, ammonium persulphate/sulfuric acid, Potassium Persulphate/sulfuric acid, iron(ic) chloride/hydrochloric acid, chromic acid, chromic acid/hydrochloric acid, potassium bichromate/sulfuric acid and iron stearate (III) salt.
Aspect the of the present invention the 42, a kind of instrument according to above-mentioned the 40 aspect is provided, it is characterized in that: above-mentioned oxidation retarder is selected from: the 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
Aspect the of the present invention the 43, a kind of instrument according to above-mentioned the 40 aspect is provided, it is characterized in that: above-mentioned additive is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, Duponol SP and Duponol WN.
Aspect the of the present invention the 44, a kind of instrument according to above-mentioned the 40 aspect is provided, it is characterized in that: above-mentioned grinding and polishing dish comprises nonwoven grinding and polishing dish.
Aspect the of the present invention the 45, a kind of instrument according to above-mentioned the 40 aspect is provided, it is characterized in that: during above-mentioned CMP handled, above-mentioned slurry was below 100 temperature.
Aspect the of the present invention the 46, provide a kind of speed of removing that carry out the CMP processing with the grinding and polishing dish during, improves material to make the minimized method of depressionization simultaneously, this method comprises makes described material contact with the slurry of claim 1, and carries out temperature maintenance that above-mentioned CMP handles and will begin the temperature of being out of shape significantly being lower than the grinding and polishing dish.
Aspect the of the present invention the 47, a kind of method according to above-mentioned the 46 aspect is provided, it is characterized in that: above-mentioned grinding and polishing dish comprises nonwoven grinding and polishing dish.
In the 40 eight aspect of the present invention, a kind of method according to above-mentioned the 46 aspect is provided, it is characterized in that: said temperature is lower than 100 °F.
Aspect the of the present invention the 49, a kind of method according to above-mentioned the 46 aspect is provided, it is characterized in that: above-mentioned materials comprises copper or copper alloy.
Aspect the of the present invention the 50, a kind of method according to above-mentioned the 46 aspect is provided, it is characterized in that: above-mentioned slurry comprises etching reagent, oxidation retarder and additive, this additive is regulated the cooperation between copper and the oxidation retarder significantly.
Of the present invention above and other aspect, by reading following will do clearer that be described in detail of the present invention, in the following description, be referring to following accompanying drawing:
The sectional view of Fig. 1 has illustrated the substrate that has the copper layer above that, and this copper layer is handled with CMP technology of the present invention.
Fig. 2 is the schematic diagram that is used for finishing the CMP instrument of art breading of the present invention.
Preferred embodiment
As shown in Figure 1 of this application, oxide compound 10 has the wide opening 14 of narrow opening 12 and formation metal wire.Each opening all uses lining (liner) 20 and copper 22 to fill.In the present invention, the part of metal level 22 (dotting) is formed on the upper surface of lining 20 and will be removed with the CMP method by grinding and polishing slurry of the present invention, and the result forms final upper surface 22A.
During carrying out this processing, reach 4 purposes: the high chemical machinery of copper 22 is removed speed; The low speed of removing of lining material 20; The low speed of removing of lower floor's dielectric layer 10; With the corrosion that prevents copper.Obviously, a purpose is that the speed of removing of copper is maximized, and can handle many more wafers because grinding and polishing was handled in the fast more then unit time, and will reduce the cost of entire semiconductor device.The 2nd purpose is during copper CMP is handled the speed of removing of lining 20 to be minimized, the step that provides a good grinding and polishing of confession to stop, and make copper in groove 14 internal loss minimums.As shown in Figure 1, this loss of metal is typically said and is counted as a kind of ' depressionization (dishing or dish typeization) '.As the 3rd purpose, because as a kind of practicable situation, lining might have some loss, particularly on the special angle of groove 14, people require the speed of removing of the dielectric layer 10 that comes out is minimized.The too much sub-cloud dielectric medium that removes will cause the nonplanarity on final surface, and this nonplanarity will cause difficulty in back to back step.At last because copper is highly corrosion-prone, still need guarantee that any corrosive factor of removing processing all is reduced to minimum.Four purposes of this of copper CMP facture (height of copper is removed speed, and can significantly not remove sub-cloud lining and dielectric medium, and, do not have obvious corrosion) usually can not get both.For example, in existing technology, usually sacrifice the speed of removing of massive material, so that prevent removing of excessive lining.Under the corrosive cost of the excessive depressionization of figure or copper, can obtain the ratio of massive material higher remove speed.
As shown in Figure 1, in the present invention, the thickness of lining 20 is the order of magnitude of 40nm, and is made of tantalum.Surrogate comprises other tantalum alloy, such as tantalum nitride and other refractory metal and refractory metal alloy, such as tungsten, chromium and titanium/titanium nitride.A kind of blocking layer based on Ta shows the best of breed that following aspect is provided: (a) promote the bonding of copper and oxide skin 10, (b) prevent the diffusion of copper, the silicon circuit of the diffusion couple lower floor of copper will have deleterious electrical effect, (C) during CMP handles, copper is provided the selectivity of removing speed.Then, copper 22 is deposited to the wafer top, and thickness (recording to the upper surface of copper layer from the upper surface of oxide skin 10) is similar to 1 micron.The copper layer can form with any depositing technics, but this technology groove in the fill oxide layer 10 and do not form the space fully.
Remove the copper layer to remove a part of metal level that is positioned on the passivation layer upper surface, so that form smooth surface by CMP then.In fact, as shown in Figure 2, the workpiece of Fig. 1 is placed on carrying of CMP instrument T and holds within the device C.Many known CMP instruments any comprises the instrument that can buy from IPEC Corp. and Strasbaugh Corp., can be used for finishing CMP operation of the present invention.CMP instrument T has grinding and polishing wheel (or platen) PL of a rotation, and a grinding and polishing dish P is housed above that.CMP slurry of the present invention is added on the grinding and polishing dish P by nozzle N, carries to hold device C wafer is contacted with grinding and polishing dish P.In fact, carry and to hold device C and on the R1 direction, rotate, with the sense of rotation R2 complementation of grinding and polishing wheel.In the operating period of the following stated, say that typically the grinding and polishing wheel is to be close to the speed rotation of a per minute 40-100 cycle (RPM), the wafer retainer is then to be close to the speed rotation of 20-100RPM.In addition, the wafer retainer adds that also pressure P R is loaded with carrying of wafer and holds device C and cling on the grinding and polishing dish P to force.The dish of urethane dish (such as the IC1000 available from Rodel), foam panel (such as the Politex available from Rodel) and other type also can use together with slurry, but, the inventor finds, can optimize whole result in this application such as those nonwoven dishes available from Freudenberg or Thomas West Inc..In the described operation of bottom, added pressure P R is close to 3-6 pound (PSI) per square inch.In fact, these 3 variablees (speed of rotation of the speed of rotation of wafer retainer, grinding and polishing dish and pressure) are relative to each other, and can and really as for example being changed by the hardness of the layer of grinding and polishing and the function of thickness.
In slurry of the present invention, in reaction, use such as having the aggregate diameter to strengthen physical abrasion at the solid that is close to 0.3 micron or the following aluminium oxide particles, excessive scratch or other surface damage are minimized.This slurry comprises following component:
1) a kind of etching reagent that promotes the copper oxidation is such as iron nitrate and compound, hydrogen peroxide, Potassium Iodate, manganese oxide, ammonium hydroxide, ammonium persulphate, Potassium Persulphate, ammonium persulphate/sulfuric acid, Potassium Persulphate/sulfuric acid, iron(ic) chloride/hydrochloric acid, chromic acid, chromic acid/hydrochloric acid, potassium bichromate/sulfuric acid and iron stearate (III) salt thereof.
2) a kind of by means of reacting the inhibitor that prevents copper dissolution with the copper surface, such as the various benzotriazole cpds of selling with trade(brand)name ' BTA ' (1-H benzotriazole for example, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole).
3) additive formed of a kind of mixture of the sodium salt by sulfated fatty alcohol, the response location of this additive and BTA contention Cu to be slowing down the growth of Cu-BTA film, and as wetting agent, as will at length discussing in bottom.
Before at length telling about technological process, investigate earlier the chemical reaction that will optimize prevailingly.In the present invention, the CMP of copper comprises steady-state process in general, by means of this process, copper be exposed in a kind of oxygenant in above-mentioned (1 and 2), enumerated and the inhibitor during will form few several unimolecular layer Cu-BTA films (when iron nitrate as oxygenant and benzotriazole during as inhibitor, the order of magnitude of the thickness of this Cu-BTA film is 14 dusts).Uncontrollable rapidly-soluble this Cu-BTA film that prevents copper is removed (promptly adopting the solia particle in the CMP slurry) with the way of physical abrasion then.Along with the 1st unimolecular layer is removed, by the said reaction in top, the copper that is come out will form new Cu-BTA unimolecular layer.With regard to complanation, this process is very fast to the higher part ratio of the ratio of Cu layer in essence, because the grinding and polishing dish of CMP instrument gives the higher part of such ratio with bigger pressure, promote the physical abrasion part of this reaction, and in the lower part of Cu layer, physical abrasion there is smaller, thereby reaction makes progress slowly till the upper surface of Cu layer becomes a plane (thereby the pressure that is equated from the grinding and polishing dish) there.This circulation of wearing and tearing/dissolving/passivation is proceeded till the part at the tantalum layer on the upper surface of passivation 10 20 comes out.Above-mentioned circulation must be optimized for correct speed to be carried out.If the Cu-BTA speed of response is high also to have formed thick Cu-BTA layer, then CMP removes speed and reduces.Under the situation of very slow speed of reaction, people will emit the danger of corrosion (not controllably dissolving) copper-connection.For the Cu-BTA that weares and teares, used a kind of aluminum oxide (Al
2O
3) aqueous colloid suspension.Find to have the use of the colloidal alumina (and a nonwoven grinding and polishing dish is just as following will discussion) of little particle size, reduced the scratch of soft copper interconnection.In order to strengthen dielectric the remove speed of copper metallographic phase, make slurry maintain low PH (at the order of magnitude of 1.2-2.5) for lower floor.
The inventor finds, E.I.Du Pont Company the additive of sodium salt mixt of sulfated fatty alcohol of a kind of commodity Duponol SP by name be absolutely necessary for the performance that strengthens slurry.Duponol SP is also known with the Empimin LV33/A of Supralate SP, the Albright of Witco Corporation and Wilson Americas Inc..Though existing technology utilizes tensio-active agent to promote CMP slurry colloidal suspensionization, in the present invention, use the CMP that additive strengthens copper and remove speed.In the present invention's prescription, keep the suspension of slurry by mechanical stirring, rather than adopt the interactional way of tensio-active agent/aluminum oxide.Tensio-active agent disclosed herein is the anion surfactant that tensio-active agent that a kind of ratio is used in the example of people's such as above-mentioned Luo article has obviously shorter chain length and lower molecular weight.People's such as Luo article has been reported and has been used a kind of nonionic surface active agent poly-(ethylene glycol), and the order of magnitude of its molecular weight is 100 ten thousand, so that promote slurry to suspend by Coulomb repulsion.Poly-(ethylene glycol) use (MW=10000) of the lower molecular weight that people such as Luo find is invalid keeping aspect the slurry suspension.
When uses such as the inventor did not contain the aluminum oxide of Duponol/BTA/ iron nitrate slurry, though abradant still is maintained suspension, the CMP of Cu removed speed but less than the 50nm/ branch.Have only to have added after the Duponol SP, CMP removes speed just will rise to intimate 300nm/ branch, and this is good for improving semiconducter device manufacturing efficient.The inventor believes that Duponol SP and BTA at copper surface competitive adsorption device, therefore, have limited the whole thickness of copper-BTA upper layer, thereby caused removing viewed increase on the speed at CMP.In general, the effect of Duponol SP is significantly to regulate the Cu-BTA complex reaction, and it is carried out with correct speed, so that make the whole speed maximization of copper polishing, corrosion is delayed.Should also be noted that owing to its low relatively molecular weight Duponol SP is being effectively aspect the minimizing solution surface tension.In the time of in being included in the copper slurry, it will increase slurry/grinding and polishing disc system to the copper wettability of the surface, and further improve polishing speed.
At Merck Index (Eleventh Edition, S.Budavari, Ed.Publ.Merck﹠amp; Co.Inc., Rahway, N.J., p.683 (1989)) in, Duponol is described to the sodium salt mixt ' Gardinol type washing composition ' by the sulfated fatty alcohol of the mixed fatty acid manufacturing of reduction Oleum Cocois or cotton seed oil and fish oil.So, it has the Probability Distribution of certain hydrocarbon chain length (C8-C18), and 8 carbon atom chain length are main ingredients in Duponol SP.Find that also pure sodium octyl sulfate (CH3) (CH2) CMP that 70SO3Na (numeral is a subscript) also can Reinforced Cu is removed speed, although than the needed concentration height of Duponol SP.Should be understood that pure alkyl-sulphate is more more expensive significantly than its ' natural ' counterpart, thereby actual value is lower in production environment.The feature of sodium octyl sulfate is: (in H2O, under 40 ℃, CMC=1.4 * 10-1M), wherein CMC is a concentration, and the colloid bundle of accumulative surfactant molecule (micella) begins to form under this concentration to have high relatively micelle-forming concentration.High CMC meaned before micella begins to form, and can reach copper/grinding and polishing dish intersection than higher monomer concentration, therefore can regulate the formation of Cu-BTA film better.In addition, because it is to help for reducing intersection tension force and single polymers form of improving wettability, so wish the tensio-active agent of high CMC.The Duponol concentration of using in slurry of the present invention is estimated identical with CMC or lower, so that can not form the micella of considerable amount.
Based on above-mentioned, the inventor believes, remove outside Duponol SP and the pure sodium octyl sulfate, other fatty alcohol vitriol (ester) tensio-active agent also can use, as long as this tensio-active agent has low relatively molecular weight (less than about 350) and has high relatively CMC.Some example comprises the derivative of sodium octyl sulfate and longer chain, the sodium octyl and the derivative of long-chain more, also be known as available from the Supralate WN of Witco Corp. or available from Albright and Wilson Americas the Empicol LB33/A of Inc with the Duponol WN.Duponol WN that is the mixture of a kind of octyl group and sodium decyl sulfate.
In addition, the inventor finds that also this slurry is not removed the tantalum layer 20 or the oxide compound 10 of sub-cloud significantly.Cu remove speed be 300nm/ divide the order of magnitude time, it is 100: 1 the speed ratio of removing that above-mentioned slurry also produces the order of magnitude for the lining of lower floor, removes speed ratio for the oxide compound of lower floor and has then surpassed 100: 1.Under high alumina concentration (3% solid), can observe 50: 1 above copper CMPs for above-mentioned materials and remove speed ratio even.Particularly the inventor finds, the application of colloidal alumina particulate has strengthened the rate selection of removing of the relative tantalum lining layer of copper widely.Though other particulate (such as colloid silica) does not have the tantalum base film that selectively wears away copper and lower floor,, as mentioned above, discoveries such as the inventor have the above-mentioned slurry of alumina particulate and do not attack tantalum significantly.
Discoveries such as the inventor make depressionization minimum in order to make the copper removal rates maximum simultaneously, and controlled temperature is important during grinding and polishing is handled.Say in more detail, the carrying out that discoveries such as the inventor are handled along with grinding and polishing, the chemical composition of the temperature-activated of the inherent frictional force in handling owing to grinding and polishing and the copper complex reaction of above explanation, the temperature of slurry can rise.Discoveries such as the inventor surpass about 100 °F if temperature rises to, and then will produce the depressionization of graphical wide line, because grinding and polishing dish deliquescing and begin distortion, and the etching increase handled of chemical composition/CMP at one time.In fact, this temperature control utilizes water-cooled grinding and polishing platen to realize.
Embodiment 1
The workpiece for preparing like that as mentioned above is to carry out grinding and polishing 0.3 micron or the following colloidal alumina dispersion liquid (for example, can buy from Cabot Corporation and other supplier) there having the particle size order of magnitude.This particle size can be removed speed and reduce removing of block film in Reinforced Cu provides optimum balance between the speed, also will reduce the scratch to the Ta film simultaneously.This slurry comprises 18 liters of deionized waters (0.3% aluminum oxide), 1.2 grams per liters (grams per liter) BTA, and 22 grams per liter iron nitrates and 3 milliliters/rise Duponol SP, make overall slurry have about 1.5 PH.The resulting speed of removing is approximately the 300nm/ branch, and for the Ta of lower floor layer, removing speed ratio is 100: 1.
Embodiment 2
The workpiece that like for preparing as mentioned above as mentioned above, is to carry out grinding and polishing in 0.3 micron or the following colloidal alumina dispersion liquid having the particle number magnitude.Slurry comprises 18 liters of deionized waters.In a series of experiments,
1) BTA, the concentration of iron nitrate and Duponol SP remains constant, and aluminum oxide solid per-cent changes between 0.1% to 3%, and Cu is removed speed or the not obviously influence of Ta selectivity.When having surpassed about 3% solid, the selectivity of Ta is just begun to reduce, although the amount that reduces is lower.Based on this result, suppositions such as the inventor, (0.3% is counted as maximum selectivity, simultaneously also the most cheap, because the % solid that is increased can increase the whole price of slurry) selectivity remains acceptable till near 15% solid.
2) percentage ratio of aluminum oxide solid, iron nitrate and Duponol SP concentration remains constant, and the amount of BTA then changes between 0.1 grams per liter and 4 grams per liters.The Cu corrosion takes place when 0.5 grams per liter is following.And between about 0.5 grams per liter and 3 grams per liters the time, it is quite uniform that Cu CMP removes speed.When having surpassed 3 grams per liters, remove speed and begin to reduce.
3) percentage ratio of aluminum oxide solid, BTA and Duponol SP concentration remains constant, and the concentration of iron nitrate changes between 40 grams per liters at 2 grams per liters.When about 2 grams per liters were following, Cu removed speed and descends exponentially, remove speed when surpassing about 2 grams per liters and then rise linearly, when about 25 grams per liters are above, remove speed there is no significant increase and
4) percentage ratio of aluminum oxide solid, BTA and iron nitrate concentration remains constant, and the change in concentration of Duponol SP.Below 3 milliliters/liter the time, the CMP of Cu removes speed and reduces about, and viewed etch rate does not significantly change under higher Duponol SP concentration.
Remove outside the fine copper, the present invention also be applicable to copper alloy (for example, have various metals up to about 5%: such as Al, Sn, In, Ti, Ag, Mo, Zr, Mg, Cr, the copper of Au and Pb), wherein this copper alloy will carry out grinding and polishing according to the described reaction kinetics in top.
Should be understood that to above preferred embodiment can carry out above-mentioned and other correction and do not depart from aim of the present invention.For example, in embodiment 2, the relative concentration of the main ingredient of slurry changes individually.The inventor etc. point out that some component concentrations is directly related each other, and the concentration of other related component changes pro rata if the percentage ratio concentration of feasible a kind of component changes.As a special case, if the density loss of iron nitrate below 2 grams per liters, then the concentration of BTA will drop to the low side of the concentration range of mentioning in the foregoing description 2.
Claims (50)
1, a kind of CMP slurry that is used for grinding and polishing copper layer or copper alloy layer comprises etching reagent, oxidation retarder and additive, and this additive is regulated the cooperation between copper and the oxidation retarder significantly.
2, the described slurry of claim 1, it is characterized in that: above-mentioned etching reagent is selected from: iron nitrate and compound thereof, hydrogen peroxide, Potassium Iodate, manganese oxide, ammonium hydroxide, ammonium persulphate, Potassium Persulphate, ammonium persulphate/sulfuric acid, Potassium Persulphate/sulfuric acid, iron(ic) chloride/hydrochloric acid, chromic acid, chromic acid/hydrochloric acid, potassium bichromate/sulfuric acid and iron stearate (III) salt.
3, the described slurry of claim 1, it is characterized in that: above-mentioned etching reagent comprises iron nitrate.
4, the described slurry of claim 1, it is characterized in that: above-mentioned oxidation retarder is selected from: 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2 OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
5, the described slurry of claim 1, it is characterized in that: above-mentioned oxidation retarder comprises BTA.
6, the described slurry of claim 1, it is characterized in that: above-mentioned additive comprises the sodium salt of sulfated fatty alcohol.
7, the described slurry of claim 6 is characterized in that: above-mentioned sodium salt has the molecular weight less than about 350.
8, the described slurry of claim 6, it is characterized in that: above-mentioned sodium salt does not form the micella that is higher than micelle-forming concentration.
9, the described slurry of claim 7, it is characterized in that: the sodium salt of above-mentioned sulfated fatty alcohol is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, Duponol SP and Duponol WN.
10, the described slurry of claim 1, it is characterized in that: above-mentioned additive comprises DuponolSP.
11, the described slurry of claim 1 is characterized in that: also comprise colloidal alumina.
12, the described slurry of claim 11 is characterized in that: above-mentioned colloidal alumina has particle diameter less than about 0.3 micron particulate.
13, the described slurry of claim 1, it is characterized in that: above-mentioned slurry has the PH of 1.2-2.5.
14, a kind of CMP slurry of grinding and polishing that be used at the copper layer or the copper alloy layer of lining top, this slurry provides the 1st of above-mentioned copper or copper alloy to remove speed, remove speed with the 2nd of above-mentioned lining, the above-mentioned the 1st removes speed, and to remove speed than the above-mentioned the 2nd at least big 50 times, this slurry comprises etching reagent, oxidation retarder and additive, and this additive is regulated the cooperation between copper and the oxidation retarder significantly.
15, the described slurry of claim 14, it is characterized in that: above-mentioned etching reagent is selected from: iron nitrate and compound thereof, hydrogen peroxide, Potassium Iodate, manganese oxide, ammonium hydroxide, ammonium persulphate, Potassium Persulphate, ammonium persulphate/sulfuric acid, Potassium Persulphate/sulfuric acid, iron(ic) chloride/hydrochloric acid, chromic acid, chromic acid/hydrochloric acid, potassium bichromate/sulfuric acid and iron stearate (III) salt.
16, the described slurry of claim 15, it is characterized in that: above-mentioned etching reagent comprises iron nitrate.
17, the described slurry of claim 14, it is characterized in that: above-mentioned oxidation retarder is selected from: 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2 OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
18, the described slurry of claim 14, it is characterized in that: above-mentioned oxidation retarder comprises BTA.
19, the described slurry of claim 14, it is characterized in that: above-mentioned additive comprises the sodium salt of sulfated fatty alcohol.
20, the described slurry of claim 19 is characterized in that: above-mentioned sodium salt has the molecular weight less than about 350.
21, the described slurry of claim 20, it is characterized in that: above-mentioned sodium salt does not form the micella that is higher than micelle-forming concentration.
22, the described slurry of claim 20, it is characterized in that: the sodium salt of above-mentioned sulfated fatty alcohol is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, Duponol SP, Duponol WN.
23, the described slurry of claim 14, it is characterized in that: above-mentioned additive comprises DuponolSP.
24, the described slurry of claim 14 is characterized in that: also comprise colloidal alumina.
25, the described slurry of claim 24 is characterized in that: above-mentioned colloidal alumina has particle diameter less than 0.3 micron particulate.
26, the described slurry of claim 14, it is characterized in that: above-mentioned slurry has the PH for 1.2-2.5.
27, a kind of grinding and polishing that is used for is in the copper layer of lining top or the slurry of copper alloy layer, the low combination of removing speed that above-mentioned slurry provides the height of above-mentioned copper or copper alloy to remove speed and above-mentioned lining, and comprise acid attack agent, oxidation retarder, colloidal alumina and sulfated fatty alcohol tensio-active agent.
28, the described CMP slurry of claim 27 is characterized in that: above-mentioned colloidal alumina accounts for the 0.3-3 weight % of above-mentioned slurry.
29, the described CMP slurry of claim 27 is characterized in that: every liter above-mentioned slurry contains the above-mentioned acid attack agent of 2 grams at least.
30, the described CMP slurry of claim 27, it is characterized in that: every liter above-mentioned slurry contains 3 milliliters of above-mentioned tensio-active agents at least.
31, a kind ofly comprising that wafer carries the method for grinding and polishing copper in the CMP instrument of holding device and grinding and polishing dish or copper alloy, this method comprises the steps:
The wafer that has the copper layer on the surface thereon is placed into wafer to be carried and holds in the device;
The slurry that comprises etching reagent, oxidation retarder and sulfated fatty alcohol tensio-active agent is added on the above-mentioned grinding and polishing dish, and above-mentioned tensio-active agent has the molecular weight less than 350, and regulate significantly between copper and the above-mentioned oxidation retarder cooperation and
The above-mentioned wafer of way grinding and polishing that employing makes above-mentioned copper layer contact with above-mentioned grinding and polishing dish.
32, the described method of claim 31 is characterized in that: above-mentioned slurry is added to above-mentioned steps on the above-mentioned grinding and polishing dish, is to finish before carrying the above-mentioned steps of holding on the device above-mentioned wafer being placed into above-mentioned wafer.
33, the described method of claim 31, it is characterized in that: above-mentioned etching reagent comprises iron nitrate.
34, the described method of claim 33, it is characterized in that: above-mentioned oxidation retarder is selected from: 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2 OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
35, the described method of claim 31, it is characterized in that: above-mentioned tensio-active agent comprises sulfation lipid acid.
36, the described method of claim 35 is characterized in that: above-mentioned sulfation lipid acid is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, DuponolSP and Duponol WN.
37, the described method of claim 31, it is characterized in that: above-mentioned slurry has the PH of 1.2-2.5.
38, the described method of claim 31 is characterized in that: above-mentioned grinding and polishing dish comprises nonwoven grinding and polishing dish.
39, the described method of claim 38 is characterized in that: above-mentioned grinding and polishing step is carried out under the also low temperature of the temperature of being out of shape significantly than above-mentioned nonwoven grinding and polishing dish.
40, a kind of instrument that the copper on the blocking layer top that is configured in the workpiece top or copper alloy are carried out CMP of being used for, it comprises:
A wafer that is used for keeping wafer carries and holds device;
One carries with wafer in CMP operating period and to hold the grinding and polishing dish that the wafer in the device contacts;
A kind of slurry, this slurry provides the 1st of above-mentioned copper or copper alloy to remove speed, remove speed with the 2nd of above-mentioned blocking layer, the above-mentioned the 1st removes speed, and to remove speed than the above-mentioned the 2nd at least big 50 times, this slurry comprises etching reagent, oxidation retarder and additive, and this additive is regulated the cooperation between copper and the oxidation retarder significantly.
41, the described instrument of claim 40, it is characterized in that: above-mentioned etching reagent is selected from: iron nitrate and compound thereof, hydrogen peroxide, Potassium Iodate, manganese oxide, ammonium hydroxide, ammonium persulphate, Potassium Persulphate, ammonium persulphate/sulfuric acid, Potassium Persulphate/sulfuric acid, iron(ic) chloride/hydrochloric acid, chromic acid, chromic acid/hydrochloric acid, potassium bichromate/sulfuric acid and iron stearate (III) salt.
42, the described instrument of claim 40, it is characterized in that: above-mentioned oxidation retarder is selected from: 1-H benzotriazole, 1-OH benzotriazole, 1-CH3 benzotriazole, 5-CH3 benzotriazole, benzoglyoxaline, 2 OH, 2-methyl-benzoglyoxaline, 5-Cl benzotriazole.
43, the described instrument of claim 40, it is characterized in that: above-mentioned additive is selected from: the sodium octyl sulfate and the derivative of long-chain more, the sodium octyl and the derivative of long-chain more, Duponol SP and Duponol WN.
44, the described instrument of claim 40 is characterized in that: above-mentioned grinding and polishing dish comprises nonwoven grinding and polishing dish.
45, the described instrument of claim 40 is characterized in that: during above-mentioned CMP handled, above-mentioned slurry was below 100 temperature.
46, a kind of speed of removing that improves material carry out the CMP processing with the grinding and polishing dish during makes the minimized method of depressionization simultaneously, this method comprises makes described material contact with the slurry of claim 1, and carries out temperature maintenance that above-mentioned CMP handles and will begin the temperature of being out of shape significantly being lower than the grinding and polishing dish.
47, the described method of claim 46 is characterized in that: above-mentioned grinding and polishing dish comprises nonwoven grinding and polishing dish.
48, the described method of claim 46 is characterized in that: said temperature is lower than 100 °F.
49, the described method of claim 46, it is characterized in that: above-mentioned materials comprises copper or copper alloy.
50, the described method of claim 46, it is characterized in that: above-mentioned slurry comprises etching reagent, oxidation retarder and additive, this additive is regulated the cooperation between copper and the oxidation retarder significantly.
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| JP2003257910A (en) * | 2001-12-28 | 2003-09-12 | Fujikoshi Mach Corp | Method for polishing copper layer of substrate |
| CN100429043C (en) * | 2003-12-29 | 2008-10-29 | 中芯国际集成电路制造(上海)有限公司 | Chemical and mechanical grinding method for aluminium |
| KR100672940B1 (en) * | 2004-08-03 | 2007-01-24 | 삼성전자주식회사 | Metal slurry for cmp and metal cmp method using the same |
| US9914852B2 (en) * | 2014-08-19 | 2018-03-13 | Fujifilm Planar Solutions, LLC | Reduction in large particle counts in polishing slurries |
| CN104716090B (en) * | 2015-03-16 | 2017-07-18 | 中国航天科技集团公司第九研究院第七七一研究所 | A kind of TSV wafer surface polishing method |
| CN109604126B (en) * | 2018-10-31 | 2021-12-10 | 博罗县东明化工有限公司 | Aluminum alloy spraying pretreatment method |
| US10964549B2 (en) * | 2018-11-30 | 2021-03-30 | Taiwan Semiconductor Manufacturing Company Limited | Wafer polishing with separated chemical reaction and mechanical polishing |
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