CN102586783B - Corrosion inhibitor, preparation method thereof and chemico-mechanical polishing composition - Google Patents
Corrosion inhibitor, preparation method thereof and chemico-mechanical polishing composition Download PDFInfo
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Abstract
The invention provides a new azol- and keto-containing corrosion inhibitor shown as a structural formula (I), and also provides a preparation method for the corrosion inhibitor and an acid chemico-mechanical polishing composition containing the corrosion inhibitor. The corrosion inhibitor is suitable for low pressure chemico-mechanical polishing compositions for multi-layer copper interconnection of very large scale integrated circuits, can quickly forms a film on the surface of copper to protect the surface of copper and inhibit corrosion, obviously reduces defects such as chemical corrosion pits, and improves the performance of a polishing solution. In the formula, R1 refers to triazolyl or tetrazolyl.
Description
Technical field
The present invention relates to chemically machinery polished waterborne compositions field, the chemical-mechanical polishing compositions that especially relates to novel corrosion inhibitor in composition and preparation method thereof and contain this inhibiter.
Background technology
Chemically machinery polished (CMP) technology is the Technology of the realization overall situation leveling that last century, the eighties was researched and developed by IBM, it can avoid defect successively stack with the increase of the interconnection number of plies, has already become the core microprocessing of nearly all step in the microelectronics production at present.
Along with integrated circuit technique enters into deep-submicron, the interconnection performance of being brought by continuous down feature sizes reduces more and more obvious.This is that the ghost effect that resistance, electric capacity, inductance cause will have a strong impact on the performance of circuit because dwindling of characteristic dimension will cause reducing of interconnecting line cross section and distance between centers of tracks.Adopting medium with low dielectric constant material (being low k dielectric materials) is one of effective way improved the interconnection performance.But, when k<2.2, the physical strength of low k dielectric layer descends, be prone to low k film delamination, so the low pressure polishing technology must be developed and polishing composition adapts to new need of production.Generally, reducing overdraft can have a negative impact to the CMP overall performance that comprises polishing speed.For example, adopt ripe commercial copper polishing composition to carry out the copper polishing, when pressure is 5.0psi, polishing speed is 333.3nm/min, and when pressure is reduced to about 0.5psi, polishing speed is decreased to 101.9nm/min, differs 3 times of left and right.Therefore, reduce the press polish meeting serious affect throughput.
Chemical-mechanical polishing compositions is a kind of important influence factor in the CMP step.Can regulate polishing performance as metal inhibitor etc. according to the oxygenant of choosing, abrasive material and other applicable additive, with the polishing speed by required, provide effective polishing, surface imperfection, corrosion are down to minimumly simultaneously, and obtain best complanation effect.CN201110065350.2 provides and has been applicable under the overdraft that at least is less than 1.0psi (6.89kPa) waterborne compositions of copper on polishing of semiconductor wafers, contain the sour corrosion poiser be applicable in the weak mechanical effect situation of low overdraft, polish removal rate reaches as high as 1711.4nm/min, and surfaceness can be to 0.30～0.95nm.U.S. Rhom and Hass has proposed a kind of composition of the low downforce pressure polishing for copper and method (CN1644644A), be applicable to the copper on polishing of semiconductor wafers under the overdraft that at least is less than 3.0psi, the P contained compound wherein added can increase the removal of copper, under 1.0psi pressure, add ammonium phosphate front and back polish removal rate and be respectively 150.0nm/min and 266.3nm/min in embodiment.US6,620,037 adopts the polishing composition that does not add inhibiter (as BTA) to carry out the copper polishing to promoting polishing speed, yet said composition still needs 3.0psi or larger overdraft in order to effectively remove copper (during 3.0psi, polishing speed is 234.6nm/min).
The copper inhibitor of selecting in polishing fluid mostly is the azole inhibitor, comprises benzotriazole (BTA), sulfydryl benzotriazole (MBT), tolytriazole (TTA).But these inhibiter mostly have the preparation of being difficult for, the shortcoming of not environmental protection of contaminate environment, and mostly only be useful in the polishing under normal pressure.Therefore need to provide a kind of new inhibiter, better for hanging down chemically machinery polished (CMP) technology of overdraft.
Summary of the invention
In order to realize above-mentioned at least one goal of the invention, one aspect of the present invention provides a kind of new, inhibiter that contain azoles base and ketone group.Further, the present invention also provides the preparation method of this inhibiter.
On the other hand, the invention provides the chemical-mechanical polishing compositions that contains above-mentioned inhibiter.
Particularly, according to the embodiment of one aspect of the invention, inhibiter provided by the invention, its structural formula is as follows:
R
2=H ,-OH ,-(CH
2)
ncH
3, the integer that wherein n is 0-4.
Further, the present invention also provides the preparation method of above-mentioned inhibiter, comprise the steps: take that dehydrated alcohol is as solvent, take amino azole compound, aromatic aldehyde, acetone is raw material, three's mol ratio is 1: 1.2: 1.2, react under the condition of pH value 2-3, generate and there is inhibiter as claimed in claim 1.
In anhydrous ethanol solvent, under sour environment, three class raw material generation Mannich reactions, generate the compound with the disclosed structure of the present invention.
One of according to the embodiment of the present invention, above-mentioned amino azole compound is selected from the 5-amino tetrazole, the composition of 3-aminotriazole and their arbitrary proportions.
According to one of another embodiment of the present invention, the structural formula of above-mentioned aromatic aldehyde is as follows:
R wherein
3=H ,-OH ,-(CH
2)
ncH
3, the integer that n is 0-4, its position is in ortho position, contraposition, a position of aldehyde radical.
Embodiment according to a further aspect of the invention, the present invention also provides the chemical-mechanical polishing compositions that comprises above-mentioned inhibiter, comprises colloid SiO
2abrasive material 1-20wt%, oxygenant 0.5-10wt%, complexing agent 0.1-10wt%, inhibiter as claimed in claim 1, pH adjusting agent and water.Wherein: oxygenant can be inorganic or organic peroxy compound, in its compound molecule containing at least one peroxy-radical or for containing any in the compound in the high oxidation state element or more than one mixture.PH adjusting agent is selected from the group that comprises inorganic acid alkali, organic acids and base.Complexing agent is selected from the group that comprises Padil, L-Ala, L-glutamic acid, proline(Pro), hydroxyglutamic acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, Amino Trimethylene Phosphonic Acid, 2-HPAA, acetic acid, oxalic acid, citric acid, oxamide or the composition of their arbitrary proportions.The concentration range of inhibiter is 0.01-5wt%.Described composition is acid, and its pH value is 2-7, is preferably the pH value for 3-5.Water is deionized water or distilled water.
One of according to the embodiment of the present invention, the concentration of described inhibiter is preferably 0.01-0.5wt%.
According to another embodiment of the present invention, abrasive material is colloid silica, and content is 3-5wt%, and mean particle size is the 10-200 nanometer.Further, mean particle size is preferably the 50-80 nanometer.
According to another embodiment of the present invention, described oxygenant is hydrogen peroxide, and content is 0.9-3wt%.
According to another embodiment of the present invention, described complexing agent is Padil, and content is 0.5-3wt%.
According to another embodiment of the present invention, described pH adjusting agent is selected from the group that comprises sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, potassium hydroxide, ammoniacal liquor, thanomin, trolamine and the composition of their arbitrary proportions.
Technique effect of the present invention is as follows:
1. inhibiter disclosed by the invention, be adapted at using in the low piezochemistry mechanical polishing composition of multilayer copper wire in large scale integrated circuit copper, can be rapidly at the copper surface filming; protection copper surface; suppress corrosion, significantly reduce the defects such as chemical corrosion hole, improve the performance of polishing fluid.
2. the preparation method of inhibiter provided by the invention, simple, and yield is high.The product corrosion mitigating effect is good.
3. experiment showed, chemical-mechanical polishing compositions provided by the invention, be low to moderate in the overdraft situation of 2.0psi, add rear polish removal rate to reach as high as 479.86nm/min, surfaceness can be low to moderate 1.00nm.
The aspect that the present invention is additional and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
The accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become from the following description of the accompanying drawings of embodiments and obviously and easily understand, wherein:
Fig. 1 does not add metallic surface pattern 3-D view after the copper polishing fluid polishing of inhibiter;
Fig. 2 adds metallic surface pattern 3-D view after the copper polishing fluid polishing of benzotriazole (BTA);
Fig. 3 is the copper polishing fluid surface of polished pattern 3-D view that adds 4-OH 4TP of the present invention.
Embodiment
Below describe embodiments of the invention in detail, the example of described embodiment is shown in the drawings.Be exemplary below by the embodiment be described with reference to the drawings, only for explaining the present invention, and can not be interpreted as limitation of the present invention.
The preparation method of inhibiter provided by the invention, specifically comprise the steps: to calculate each raw material consumption according to amino azole compound, acetone, aromatic aldehyde ingredient proportion (mol ratio) 1: 1.2: 1.2.Using dehydrated alcohol as solvent, quantitative amino azole compound is dissolved in dehydrated alcohol to the (consumption of dehydrated alcohol, with reactant degree of being dissolved as fully) until completely dissolved, add acetone and aromatic aldehyde, regulating pH with dilute hydrochloric acid is 2-3, stir certain hour under room temperature, cooling.Churning time can be determined according to response situation, for example stirs 24h even for more time.
After question response is abundant, can, further by removal of solvents, for example can adopt Rotary Evaporators to steam solvent.And recrystallization, the number of times of recrystallization can be for repeatedly, and for example twice, obtain the target product of solid powdery.Screwing out the front product of solvent is liquid.After screwing out solvent, products therefrom becomes pressed powder.Step by recrystallization can purified product.
Below, in detail with the form of embodiment, preparation method and the corresponding product of inhibiter provided by the invention is described in detail.
Embodiment 1
At first 0.05mol 5-amino tetrazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol phenyl aldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (4TP) that Mannich base is the main body composition, and structural formula is as follows:
Embodiment 2
At first 0.05mol 5-amino tetrazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol salicylaldhyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (2-OH-4TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 3
At first 0.05mol 5-amino tetrazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol4-hydroxy benzaldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (4-OH-4TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 4
At first 0.05mol 5-amino tetrazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol p-tolyl aldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (4-Me-4TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 5
At first 0.05mol 5-amino tetrazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol p-ethylbenzaldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (4-Et-4TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 6
At first 0.05mol 3-aminotriazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol phenyl aldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (3TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 7
At first 0.05mol 3-aminotriazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol salicylaldhyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (2-OH-3TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 8
At first 0.05mol 3-aminotriazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol p-Hydroxybenzaldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (4-OH-3TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 9
At first 0.05mol 3-aminotriazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol p-tolyl aldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (4-Me-3TP) that Mannich base is the main body composition, and its structural formula is as follows:
Embodiment 10
At first the 0.05mol3-aminotriazole is dissolved in the 50-100ml dehydrated alcohol, after the question response thing dissolves fully, then adds acetone and the 0.06mol p-ethylbenzaldehyde of 0.06mol, regulating pH with dilute hydrochloric acid is 2-3, under room temperature, stirs 24h, cooling.Twice recrystallization obtains take the product (4-Et-3TP) that Mannich base is the main body composition, and its structural formula is as follows:
Comparative experimental example 1 polishing experiments and corrosion inhibition evaluation
1. experiment is divided into groups and is subject to trial product:
It is 12 groups that experiment is divided into, and wherein control group is 2 groups, and 10 groups of experimental group adopt respectively following chemical-mechanical polishing compositions:
Control group 1 adds 10 gram Padils in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Control group 2 adds 10 gram Padils, 100 milligrams of benzotriazoles (BTA) in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 1 adds 10 gram Padils, 100 milligrams of embodiment 1 gained 4TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 2 adds 10 gram Padils, 100 milligrams of embodiment 2 gained 2-OH-4TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 3 adds 10 gram Padils, 100 milligrams of embodiment 3 gained 4-OH-4TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 4 adds 10 gram Padils, 100 milligrams of embodiment 4 gained 4-Me-4TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 5 adds 10 gram Padils, 100 milligrams of embodiment 5 gained 4-Et-4TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 6 adds 10 gram Padils, 100 milligrams of embodiment 6 gained 3TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 7 adds 10 gram Padils, 100 milligrams of embodiment 7 gained 2-OH-3TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 8 adds 10 gram Padils, 100 milligrams of embodiment 8 gained 4-OH-3TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 9 adds 10 gram Padils, 100 milligrams of embodiment 9 gained 4-Me-3TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
Experimental group 10 adds 10 gram Padils, 100 milligrams of embodiment 10 gained 4-Et-3TP in 800 gram deionized waters, stirring and dissolving, evenly after, slowly stir the 50 nano silicon water-sols that add 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2sO
4calibration pH value to 4.0, finally add water and supply 1000 grams and stir, and obtains the copper polishing fluid.
2. laboratory apparatus and method: it is the polishing experiments machine that polishing experiments is used CETR CP4, use the IC1000/SUBA IV of Rodel company microvoid polyurethane polishing pad, the polishing disk rotating speed is that 100r/min, polishing fluid flow are 100mL/min, and polished is 2 cun silica-based copper sheets of electroplating surface.Static etch rate (SOR) and polish removal rate (MRR) adopt the precise electronic balance check weighing that precision is 0.01mg to calculate, and use the three-dimensional white light interference surface topographic apparatus fo of the microXAM of Veeco company to observe surface topography gauging surface roughness (Sa).
Above control group and experimental group are all carried out static corrosion experiment and dynamic polishing experiments, static corrosion time 10min, and the polishing overdraft is 2.0psi.
3. experimental result:
Experimental result is in Table 1 in detail.Fig. 1-3 are shown in by the surface of polished pattern observation schematic diagram of Comparative Examples 1, Comparative Examples 2 and embodiment 3.
The corrosion inhibition of the different inhibiter of table 1 and on the impact of polishing effect
As shown in table 1, with relatively blank sample Comparative Examples 1, compare, after adding different inhibiter, SOR and MRR all produce decline in various degree, illustrate that various inhibiter have all produced absorption film-forming on the copper surface, meet the inhibition mechanism of inhibiter.But improved greatly surface quality index S a adding of inhibiter, wherein better with OH TP series.The corrosion mitigating effect of all kinds of inhibiter of comprehensive assessment and polishing characteristic, 4-OH-4TP shows optimum, when maintaining high polishing removal, has greatly improved the polished surface quality, and surfaceness Sa is low to moderate 1.00nm.In Fig. 1-3, also can see: the silicon copper sheet surface after the polishing of interpolation inhibiter is more smooth, and cut and corrosion pit all reduce.Comparison diagram 2 and Fig. 3 can find out, by the silicon copper sheet surface ratio after the inhibiter polishing fluid polishing of adding TP series, adds more flat-satin of silicon copper sheet after the polishing of BTA polishing fluid, and corrosion pit is less.
The interpolation of inhibiter provided by the invention in the chemically machinery polished waterborne compositions, can effectively guarantee the polishing speed of wafer copper-connection polishing and promote surface quality under the low overdraft of 2.0psi, avoid to greatest extent the generation of polishing defect, can replace BTA commonly used to use in the low piezochemistry mechanical polishing waterborne compositions of copper fully.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (10)
1. an inhibiter, is characterized in that, the structural formula of described inhibiter is as follows:
R
1=
R
2=H ,-OH ,-(CH
2)
ncH
3, the integer that wherein n is 0-4.
2. the preparation method of an inhibiter, is characterized in that, described method comprises the steps:
Take dehydrated alcohol as solvent, and take amino azole compound, aromatic aldehyde, acetone is raw material, and three's mol ratio is 1:1.2:1.2, under the condition of pH value 2-3, reacts, and generates and has inhibiter as claimed in claim 1.
3. preparation method as claimed in claim 2, wherein said amino azole compound is selected from the 5-amino tetrazole, the 3-aminotriazole.
4. preparation method as claimed in claim 2, the structural formula of wherein said aromatic aldehyde is as follows:
R wherein
3=H ,-OH ,-(CH
2)
ncH
3, the integer that n is 0-4, its position is in ortho position, contraposition, a position of aldehyde radical.
5. a chemical-mechanical polishing compositions, is characterized in that, comprises colloid SiO
2abrasive material 1-20wt%, oxygenant 0.5-10wt%, complexing agent 0.1-10wt%, inhibiter as claimed in claim 1, pH adjusting agent and water, wherein
Described oxygenant is inorganic or the organic peroxy compound, in its compound molecule containing at least one peroxy-radical or for containing any in the compound in the high oxidation state element or more than one mixture;
Described pH adjusting agent is selected from the group that comprises inorganic acid alkali, organic acids and base;
Described complexing agent is selected from the group that comprises Padil, L-Ala, L-glutamic acid, proline(Pro), hydroxyglutamic acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, Amino Trimethylene Phosphonic Acid, 2-HPAA, acetic acid, oxalic acid, citric acid, oxamide or the composition of their arbitrary proportions;
The concentration of described inhibiter is 0.01-5wt%;
The pH value of described composition is 2-7; Being preferably the pH value is 3-5;
Described water is deionized water or distilled water.
6. chemical-mechanical polishing compositions as claimed in claim 5, the concentration of wherein said inhibiter is 0.01-0.5wt%.
7. chemical-mechanical polishing compositions as claimed in claim 5, wherein said abrasive material is colloid silica, and content is 3-5wt%, and mean particle size is 10-200 nanometers; Being preferably mean particle size is 50-80 nanometers.
8. chemical-mechanical polishing compositions as claimed in claim 5, wherein said oxygenant is hydrogen peroxide, content is 0.9-3wt%.
9. chemical-mechanical polishing compositions as claimed in claim 5, wherein said complexing agent is Padil, content is 0.5-3wt%.
10. chemical-mechanical polishing compositions as claimed in claim 5, wherein said pH adjusting agent is selected from the group that comprises sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, potassium hydroxide, ammoniacal liquor, thanomin, trolamine and the composition of their arbitrary proportions.
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