CN1162498C - Chemical and mechanical grinding fluid composition and its usage - Google Patents
Chemical and mechanical grinding fluid composition and its usage Download PDFInfo
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- CN1162498C CN1162498C CNB011227915A CN01122791A CN1162498C CN 1162498 C CN1162498 C CN 1162498C CN B011227915 A CNB011227915 A CN B011227915A CN 01122791 A CN01122791 A CN 01122791A CN 1162498 C CN1162498 C CN 1162498C
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Abstract
The present invention provides a composition of a chemically machinery grinding serous fluid for processing semiconductors, which comprises 70 to 99.5 wt. % of water nature medium, 0.1 to 25 wt. % of grinding particle, 0.01 to 1 wt. % of triazole composition as a corrosion inhibitor and 0.001 to 1 wt. % of water soluble chlorine ion source. During a grinding process, a compact layer which is generated on the surface of a copper thin film because of tempering treatment can be ground through by the water soluble chlorine ion in the composition of the grinding serous fluid of the present invention, and copper residual quantity after grinding can be lowered. The composition of the chemically machinery grinding serous fluid of the present invention can further contain an oxidizing agent. The present invention also relates to a method for grinding the surface of the semiconductor crystal by the composition.
Description
Invention field
The present invention relates to a kind of chemical and mechanical grinding fluid composition.Grinding milk composition of the present invention can effectively be applied to the grinding of semiconductor wafer surface.
Background technology
Cmp technology (be called for short CMP) is the planarization that the difficulty that causes photomicrography processing to be gone up focusing on because of plated film height difference when solving unicircuit and make develops.The cmp technology at first is applied in the manufacturing of 0.5 micron element on a small quantity, and along with dwindling of size, the number of plies that cmp is used is also more and more.To 0.25 micron epoch, cmp has become main flow and has been necessary planarization.Generally speaking, being used to make the Ginding process of metallic circuit, is that semiconductor crystal wafer is placed on the spin finishing platform of being furnished with grinding head, uses the grinding milk that comprises polishing particles and oxygenant in crystal column surface, grinds effect to promote.
United States Patent (USP) the 5th, 225 discloses a kind of chemical and mechanical grinding fluid No. 034, and it comprises AgNO
3, the solid abrasive material, be selected from H
2O
2, HOCl, KOCl, KMgO
4Or CH
3The oxygenant of COOOH.This grinding milk is the copper layer that is used on the polishing semiconductor wafers, to make the copper cash on the wafer.
United States Patent (USP) the 5th, 209 discloses a kind of chemical and mechanical grinding fluid that uses for No. 816 will contain the method for Al or Ti metal level polishing, and its grinding milk still comprises the H of about 0.1-20 volume % except that comprising the solid abrasive material
3PO
4H with about 1-30 volume %
2O
2
United States Patent (USP) the 4th, 959 relates to a kind of method that makes the use abrasive composition with the surface, burnished metal No. 113.This water-based abrasive composition comprises water, abrasive (CeO for example
2, Al
2O
3, ZrO
2, TiO
2, SiO
2, SiC, SnO
2And TiC), with a kind of salt, the negatively charged ion of the metallic cation of this salt containing element periodictable IIA, IIIA, IVA or IVB family and chlorion, bromide anion, iodide ion, nitrate radical, sulfate radical, phosphate radical or mistake chlorate anions.This United States Patent (USP) also teaching uses hydrochloric acid, nitric acid, phosphoric acid or sulfuric acid so that its water-based abrasive composition is deployed into pH=1-6.
United States Patent (USP) the 5th, 391 discloses a kind of abrasive composition that is used to polish the mixture of siliceous, silica or silicate for No. 258, and it still comprises hydrogen peroxide and Potassium Hydrogen Phthalate except that comprising abrasive grains.
United States Patent (USP) the 5th, 114, relate to a kind of polishing composition that is used for the polished aluminum base material for No. 437, it comprises average particle size particle size between the aluminum oxide polishing agent of 0.2 to 5 μ m and be selected from the polishing promotor of chromium nitrate (III), lanthanum nitrate, cerous nitrate (III) ammonium or neodymium nitrate.
United States Patent (USP) the 5th, 084 relates to a kind of chemical machinery polishing slurries that use for No. 071 with the method with the polishing of electronic component base material, and its employed polishing slurries comprise aluminum oxide, abrasive grains (for example, the SiO less than 1 weight %
2, CeO
2, SiC, Si
3N
4Or Fe
2O
3), as the transition metal of mill efficiency promotor sting close salt (for example, EDTA iron ammonium), and for the solvent of this salt use.
United States Patent (USP) the 5th, 336 discloses a kind of polishing composition No. 542, and it comprises alumina abrasive particles, and a sequestrant that is selected from polyamines yl carboxylic acid (for example EDTA) or its sodium or sylvite.This polishing composition can further comprise boehmite or aluminium salt.
United States Patent (USP) the 5th, 340 discloses a kind of slurries that are used for the chemical machinery polishing of tungsten for example or tungsten nitride film for No. 370, and it comprises hydroferricyanic acid potassium oxygenant, abrasive and water for the film use, and wherein these slurries have 2 to 4 pH value.
United States Patent (USP) the 5th, 516 discloses a kind of slurries that are used for chemical machinery polishing titanium film for No. 346, and it comprises concentration and is enough to Potassium monofluoride and abrasive (for example silicon oxide) with this titanium film complexing, and wherein these slurries have and are lower than 8 pH value.
WO96/16436 discloses a kind of chemical machinery polishing slurries, and it comprises abrasive grains, the molysite oxygenant that has less than 0.400 micron median size, the water-based interfacial agent suspension that reaches propylene glycol and methyl p-hydroxybenzoate.
Generally be used for promoting the salt of grinding rate to contain iron ion (Fe (NO for example
3)
3Or K
3Fe (CN)
6) or potassium ion (KIO for example
3), yet these metal ions can polluting wafer and CMP processing unitss, increase the workload of follow-up cleaning and reduce the time limit of service of CMP processing units.In addition, potassium ion has suitable mobility, penetrates dielectric layer easily, reduces the reliability of unicircuit.
In unicircuit processing, Ta or TaN film often are used to promote the tackiness of copper to insulating layer of silicon oxide, and in addition, Ta or TaN film also are used as membranous metal.In theory, Ta or TaN remove speed should with Cu to remove speed close, but the Ta metal is the metal with high resistance chemical, because it is difficult for oxidation, in copper processing, the grinding of Ta metal is to be difficult to the person of overcoming in the skill most always, simultaneously, because it is worn that barrier film is difficult to, often cause the problem of copper cash depression.
In addition, in the processing of this copper, the copper film can pass through that tempering (annealing) is handled and the cupric oxide that is easy to generation one deck densification on the copper film.And because the homogeneity question that CMP processing exists; Worn and when beginning to produce depression when the copper of wafer upper part, on the wafer of being everlasting, also unwanted copper can residually be arranged.Therefore, how to remove the copper residue fast and cave in, and the acceleration production capacity is the big problem that the CMP processing utmost point need overcome to reduce copper cash.
In sum, in the semiconductor machining skill, still urgently seek more economical, have more usefulness and can reduce the Chemicomechanically grinding composition of above-mentioned shortcoming.
Summary of the invention
The present invention provides a kind of chemical and mechanical grinding fluid composition that is used for semiconductor machining, and it comprises the aqueous medium of 70 to 99.5 weight %; 0.1 abrasive grains to 25 weight %; 0.01 to the triazolam thing of 1 weight % as corrosion inhibitor; And the soluble chloride ion source of 0.001 to 1 weight %.Institute's aqueous solution chlorion in the grinding milk composition of the present invention can be in process of lapping, the worn out tight zone that is produced in the copper film surface because of temper, and reduce copper residual quantity after grinding.Chemical and mechanical grinding fluid composition of the present invention can further comprise oxygenant.The present invention also relates to the method that said composition is used for the polishing semiconductor wafers surface.
Embodiment
Chemical and mechanical grinding fluid composition of the present invention comprises the aqueous medium of 70 to 99.5 weight % and preferred 80 to 99.5 weight %; 0.1 to 25 weight %, preferred 0.5 to 15 weight %, more preferably 0.5 to 10 weight % reaches the most preferably abrasive grains of 0.5 to 5 weight %; 0.01 to 1.0 weight %, preferred 0.01 to 0.5 weight % reaches the more preferably corrosion inhibitor of 0.05 to 0.2 weight %; And 0.001 to 1 weight %, preferred 0.01 to 0.5 weight %, more preferably the soluble chloride ion source of 0.02 to 0.1 weight %.Chemical and mechanical grinding fluid composition of the present invention can further comprise the oxygenant of 0.1 to 5 weight %.
By hereinafter learning, in the grinding milk composition, add the tight zone that chlorion can worn out copper surface and reduce the copper residual quantity according to embodiments of the invention.Any chlorine-containing compound that can in aqueous medium, dissociate chlorion, all can be used in the grinding milk composition of the present invention as the soluble chloride ion source, for example hydrogenchloride, ammonium chloride, dimethyl amine hydrochloride, Tetramethylammonium chloride and hydrochlorinate are partly blocked hydrazine etc.
According to the present invention, the employed abrasive grains of grinding milk composition can be general commercially available person, for example SiO
2, Al
2O
3, ZrO
2, CeO
2, SiC, Fe
2O
3, TiO
2, Si
3N
4Or its mixture.These abrasive grains have higher degree, high-specific surface area, and advantage such as narrow size distribution, therefore are applicable in the abrasive composition as abrasive grains.
Selecting for use of the aqueous medium of grinding milk composition of the present invention for those who familiarize themselves with the technology, is conspicuous, for example in preparation process, can make water, preferably uses deionized water so that abrasive composition is the slurries shape.
According to the present invention, the employed corrosion inhibitor of grinding milk composition is to be the triazolam thing, can be selected from benzotriazole, tricyanic acid, 1,2,3-triazoles, 3-amido-1,2,4-triazole, 3-nitro-1,2,4-triazole, 4-amido-3-diazanyl-5-thiol group-1,2, (Popeye gets (purpald to the 4-triazole
)), benzotriazole-5-carboxylic acid, 3-amido-1,2,4-triazole-5-carboxylic acid, I-hydroxybenzotriazole and nitrobenzene and triazolam; Preferably use benzotriazole.
According to the present invention, the employed oxygenant of grinding milk composition is a composition known in the cmp skill, and it can be selected from H
2O
2, Fe (NO
3)
3, KIO
3, CH
3COOOH and KMnO
4Preferably use H
2O
2
According to an advantageous embodiment of the invention, when deionized water was 80 to 99.5 weight %, the solids content of slurries was 0.5 to 15 weight %, was preferably 0.5 to 10 weight %, reached 0.5 to 5 weight % more preferably.Then each component as indicated above is imported in the high purity slurries of gained, add again acid or alkali with the pH value of control slurries between required scope.
The present invention also relates to the method on a kind of polishing semiconductor wafers surface, and it is to be included in to use on the crystal column surface according to chemical and mechanical grinding fluid composition of the present invention.
Following examples will the present invention is further illustrated, but not in order to limit the scope of the invention, modification and change that any personage who has the knack of this technology can reach easily all are covered by in the scope of the present invention.
Grind test
A. instrument: IPEC/Westech 472
B. condition: pressure: 2psi
Back pressure: 0.5psi
Temperature: 25 ℃
The speed of mainshaft: 93rpm
Platen rotating speed: 87rpm
Base pattern: IC1000, k-grv.
Slurry flow rate: 250 ml/min
C. wafer: the copper film, available from Silicon Valley Microelectonics.lnc., it is the thermal oxide of deposit 1000 silicon oxide on 8 inches Silicon Wafers, the PVD-Ta of 300 and the PVD copper film of 10000 ± 5%.
And place 100 ℃ baking oven to make temper this copper wafer.
D slurries: the slurries and the 30%H that get the embodiment gained
2O
2Evenly test after the stirring with 9: 1 volume ratios.
Grind testing process: before and after grinding, must measure the thickness of film with elcometer.Metallic membrane measures the sheet resistance of film with four-point probe, convert through following formula the thickness of film: T * R=specific resistance
Wherein T is that film thickness () and R are sheet resistance (Q/cm
2), for various metallic films, (Ω/cm) is a constant to specific resistance.
The present invention adopts the RS 75 type machines of KLA-Tencor company to measure the thickness of metal level.The measuring method of polishing speed is to record metal level thickness T with above-mentioned RS 75 type machines earlier
1, so that the grinding of gained slurries is after 1 minute among the embodiment, the Evergreen Mode1 10X type machine cleaning wafer with solid-state instrument company (Solid StateEquipment Corporation) afterwards, dries up wafer respectively.Measure the thickness T of metal level again with RS 75 type machines
2With T
1-T
2Be the polishing speed of metal level.
Embodiment 1
Prepare slurries with colloided silica as abrasive grains.
Slurries are composed as follows:
Colloided silica: 2.0 weight %;
Benzotriazole (BTA): 0.1 weight %;
All the other content are for adjusting ammoniacal liquor or the nitric acid and the deionized water of pH value.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 2
The preparation and the slurries of embodiment 1 described same composition, but additionally add the nitric acid of 0.2 weight %.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 3
The preparation and the slurries of embodiment 1 described same composition, but additionally add the phosphoric acid of 0.2 weight %.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 4
The preparation and the slurries of embodiment 1 described same composition, but additionally add the sulfuric acid of 0.2 weight %.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 5
The preparation and the slurries of embodiment 1 described same composition, but additionally add the hydrogenchloride of 0.2 weight %.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 6
The preparation and the slurries of embodiment 1 described same composition, but additionally add the ammonium chloride of 0.2 weight %.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 7
The slurries of preparation and embodiment 5 described same compositions just replace colloided silica as abrasive grains with aluminum oxide.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 8
The slurries of preparation and embodiment 5 described same compositions just are adjusted into the pH value between 5 to 6.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 9
The slurries of preparation and embodiment 5 described same compositions just are adjusted into the pH value between 2 to 3.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 10
The slurries of preparation and embodiment 5 described same compositions, just the consumption with hydrogenchloride changes 0.05 weight % into.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 11
The slurries of preparation and embodiment 5 described same compositions, just the dimethyl amine hydrochloride with 0.1 weight % replaces hydrogenchloride.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 12
The slurries of preparation and embodiment 5 described same compositions, just the Tetramethylammonium chloride with 0.1 weight % replaces hydrogenchloride.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Embodiment 13
The slurries of preparation and embodiment 5 described same compositions just partly block hydrazine with the hydrochlorinate of 0.1 weight % and replace hydrogenchloride.
The grinding rate of gained grinding milk and worn out tight zone time are as shown in table 1.
Table 1
| Embodiment | The abrasive grains kind | Solid content (weight %) | Additive and content thereof (weight %) | The pH value | The worn out tight zone time (second) | The copper grinding rate (/minute) |
| 1 | Colloided silica | 2 | Benzotriazole (0.1%) | 3-4 | Can't be worn out | 0 |
| 2 | Colloided silica | 2 | Benzotriazole (0.1%) HNO 3(0.2％) | 3-4 | Can't be worn out | 0 |
| 3 | Colloided silica | 2 | Benzotriazole (0.1%) H 3PO 4(0.2％) | 3-4 | Can't be worn out | 0 |
| 4 | Colloided silica | 2 | Benzotriazole (0.1%) H 2SO 4(0.2％) | 3-4 | Can't be worn out | 0 |
| 5 | Colloided silica | 2 | Benzotriazole (0.1%) HCl (0.2%) | 3-4 | 15 | 2730 |
| 6 | Colloided silica | 2 | Benzotriazole (0.1%) NH 4Cl(0.2％) | 3-4 | 25 | 1693 |
| 7 | Aluminum oxide | 2 | Benzotriazole (0.1%) HCl (0.2%) | 3-4 | 10 | 4270 |
| 8 | Colloided silica | 2 | Benzotriazole (0.1%) HCl (0.2%) | 5-6 | 20 | 1872 |
| 9 | Colloided silica | 2 | Benzotriazole (0.1%) HCl (0.2%) | 2-3 | 10 | 5325 |
| 10 | Colloided silica | 2 | Benzotriazole (0.1%) HCl (0.05%) | 3-4 | 15 | 4022 |
| 11 | Colloided silica | 2 | Benzotriazole (0.1%) dimethyl amine hydrochloride HN (CH 3) 2-HCl(0.1％) | 3-4 | 20 | 1677 |
| 12 | Colloided silica | 2 | Benzotriazole (0.1%) Tetramethylammonium chloride N (CH 3) 4 +Cl -(0.1％) | 3-4 | 25 | 1260 |
| 13 | Colloided silica | 2 | Benzotriazole (0.1%) hydrochlorinate is partly blocked hydrazine N 2NNH-C(＝O)NH 2·HCl (0.1％) | 3-4 | 25 | 1932 |
Annotate: (1) is known by embodiment 1-5, gets final product the tight zone of worn out copper crystal column surface behind the interpolation hydrogenchloride.
Know by embodiment 5-6 that (2) what play an important role is chlorion.
Know by embodiment 5 and 7 that (3) interpolation of chlorion all is applicable to colloided silica and the aluminum oxide lapping liquid as abrasive grains.
Know by embodiment 7-13 that (4) chlorion is the main material of worn out copper surface compact layer.
Claims (12)
1, a kind of chemical and mechanical grinding fluid composition, it comprises the aqueous medium of 70-99.5 weight %; 0.1-25 the abrasive grains of weight %; 0.01-1.0 weight % is as the triazolam thing of corrosion inhibitor; 0.001-1.0 the soluble chloride ion source of weight %, and the oxygenant of 0.1-5 weight %.
2, according to the chemical and mechanical grinding fluid composition of claim 1, wherein abrasive grains is selected from SiO
2, Al
2O
3, ZrO
2, CeO
2, SiC, Fe
2O
3, TiO
2, Si
3N
4, or its mixture.
3, according to the chemical and mechanical grinding fluid composition of claim 1, it comprises the abrasive grains of 0.5-15 weight %.
4, according to the chemical and mechanical grinding fluid composition of claim 3, it comprises the abrasive grains of 0.5-10.0 weight %.
5, according to the chemical and mechanical grinding fluid composition of claim 1, it comprises the soluble chloride ion source of 0.01-0.5 weight %.
6, according to the chemical and mechanical grinding fluid composition of claim 5, it comprises the soluble chloride ion source of 0.02-0.1 weight %.
7, according to the chemical and mechanical grinding fluid composition of claim 1, wherein said triazolam thing is selected from benzotriazole, tricyanic acid, 1,2,3-triazoles, 3-amido-1,2,4-triazole, 3-nitro-1,2,4-triazole, 4-amido-3-diazanyl-5-thiol group-1,2,4-triazole, benzotriazole-5-carboxylic acid, 3-amido-1,2,4-triazole-5-carboxylic acid, I-hydroxybenzotriazole and nitrobenzene and triazolam.
8, according to the chemical and mechanical grinding fluid composition of claim 7, wherein said triazolam thing is a benzotriazole.
9, according to the chemical and mechanical grinding fluid composition of claim 1, wherein said oxygenant is to be selected from H
2O
2, Fe (NO
3)
3, KIO
3, CH
3COOOH and KMnO
4
10, according to the chemical and mechanical grinding fluid composition of claim 9, wherein said oxygenant is H
2O
2
11, according to the chemical and mechanical grinding fluid composition of claim 1, wherein said soluble chloride ion source is selected from hydrogenchloride, ammonium chloride, dimethyl amine hydrochloride, Tetramethylammonium chloride and hydrochlorinate and partly blocks hydrazine.
12, a kind of method that is used for the polishing semiconductor wafers surface, it is included in uses on the crystal column surface as the chemical and mechanical grinding fluid composition of claim 1 to 11 in each.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011227915A CN1162498C (en) | 2001-07-25 | 2001-07-25 | Chemical and mechanical grinding fluid composition and its usage |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011227915A CN1162498C (en) | 2001-07-25 | 2001-07-25 | Chemical and mechanical grinding fluid composition and its usage |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1398944A CN1398944A (en) | 2003-02-26 |
| CN1162498C true CN1162498C (en) | 2004-08-18 |
Family
ID=4664899
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011227915A Expired - Lifetime CN1162498C (en) | 2001-07-25 | 2001-07-25 | Chemical and mechanical grinding fluid composition and its usage |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1162498C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4814502B2 (en) * | 2004-09-09 | 2011-11-16 | 株式会社フジミインコーポレーテッド | Polishing composition and polishing method using the same |
| JP5180185B2 (en) * | 2006-03-31 | 2013-04-10 | キャボット マイクロエレクトロニクス コーポレイション | Polymer inhibitors for improved planarization |
| CN101684392B (en) * | 2008-09-26 | 2015-01-28 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| CN101724347A (en) * | 2008-10-10 | 2010-06-09 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| US10407594B2 (en) | 2011-03-22 | 2019-09-10 | Basf Se | Chemical mechanical polishing (CMP) composition comprising a polymeric polyamine |
| CN106916536B (en) * | 2015-12-25 | 2021-04-20 | 安集微电子（上海）有限公司 | Alkaline chemical mechanical polishing solution |
-
2001
- 2001-07-25 CN CNB011227915A patent/CN1162498C/en not_active Expired - Lifetime
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|---|---|
| CN1398944A (en) | 2003-02-26 |
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