CN101747843A - Chemical-mechanical polishing solution - Google Patents
Chemical-mechanical polishing solution Download PDFInfo
- Publication number
- CN101747843A CN101747843A CN200810207473A CN200810207473A CN101747843A CN 101747843 A CN101747843 A CN 101747843A CN 200810207473 A CN200810207473 A CN 200810207473A CN 200810207473 A CN200810207473 A CN 200810207473A CN 101747843 A CN101747843 A CN 101747843A
- Authority
- CN
- China
- Prior art keywords
- acid
- mechanical polishing
- chemical mechanical
- polishing liquid
- amino
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 235000014987 copper Nutrition 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
Images
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- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention discloses chemical-mechanical polishing solution, containing ground particles, complexing agents, oxidants and water. The polishing solution is characterized by also containing one or more block polyether surfactants. The polishing solution can reduce the dents on the polished copper blocks and prevent local and general corrosion of the copper under the condition of keeping higher copper removal rate.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid.
Background technology
Development along with microelectronics, the very large scale integration chip integration has reached tens components and parts, characteristic dimension has entered nano level, and this just requires hundreds of procedure, especially multilayer wiring, substrate, medium in the microelectronic technique must pass through chemical-mechanical planarization.Very extensive integrated routing is just transformed to Cu by traditional Al.Compare with Al, it is low that Cu wiring has resistivity, deelectric transferred energy rate height, and RC is short time of lag, and the advantage of Cu wiring has made its alternative A1 become interconnected metal in the semiconductor fabrication.
But also copper material is not carried out plasma etching or wet etching effectively at present, so that the known technology that copper-connection fully forms in unicircuit, so the cmp method of copper is considered to the most effective processing method.The principle of work of the cmp method of copper generally is to remove copper a large amount of on the substrate surface with removing speed soon and efficiently earlier, and soft landing when soon near the blocking layer reduces removal speed and polishes remaining metallic copper and be parked in the blocking layer.At present, a series of chemical mechanical polishing slurry that is suitable for polishing Cu has appearred, as: the patent No. is US 6,616, and 717 disclose a kind of composition and method that is used for metal CMP; The patent No. is US 5,527, and 423 disclose a kind of chemical mechanical polishing slurry that is used for metal level; The patent No. is US 6,821, and 897 disclose a kind of method of using the copper CMP of polymer complexing agent; The patent No. is that CN 02114147.9 discloses a kind of polishing liquid used in copper chemical mechanical polishing technology; The patent No. is the used slurry of chemically machinery polished that CN 01818940.7 discloses copper; The patent No. is that CN 98120987.4 discloses a kind of CMP slurries manufacturing of copper and manufacture method that is used for unicircuit of being used for.But the above-mentioned polishing slurries that is used for copper uses the back substrate surface to exist the residual of defective, scuffing, pickup or copper, or the depression of polishing back copper billet is excessive, or exists problems such as part or general corrosion in the polishing process.Therefore be necessary to develop the chemical mechanical polishing slurry that is used for copper that makes new advances.
Summary of the invention
Technical problem to be solved by this invention is to have overcome the existing chemical mechanical polishing liquid that is used for polish copper, easily cause the excessive removal of substrate surface scuffing, contamination and copper billet and produce the defective of depression, keeping higher copper to remove under the situation of speed and provide a kind of, reduce the depression of polishing back copper billet, prevent the part of metallic copper and the chemical mechanical polishing liquid of general corrosion.
Chemical mechanical polishing liquid of the present invention contains one or more block polyether class tensio-active agents, abrasive grains, complexing agent, oxygenant and water.Described block polyether class tensio-active agent refers to the block polymer be made up of different polyethers.
What described block polyether class tensio-active agent was preferable is polyoxyethylene-poly-oxypropylene polyoxyethylene three block polyethers.This polyethers can be represented with following formula I:
(CH
2CH
2O)
x-(CH (CH
3) CH
2O)
y-(CH
2CH
2O)
z-OH is designated as (EO)
x(PO)
y(EO)
z
Wherein, 10≤x, y, z≤150.
What the content of described block polyether was preferable is mass percent 0.001～3%, and better is mass percent 0.001～1%.
Described abrasive grains can be the conventional abrasive grains that uses in this area, preferably is selected from silicon-dioxide, cerium dioxide, titanium dioxide and the polymer abrasive grains of silicon-dioxide, aluminium coating of silicon-dioxide, aluminum oxide, adulterated al such as polystyrene, the polymethylmethacrylate one or more.That the particle diameter of abrasive grains is preferable is 20～150nm, and that better is 30～120nm.What the content of described abrasive grains was preferable is mass percent 0.1～5%, and better is mass percent 0.1～3%.
Described oxygenant can be the conventional oxygenant that uses in this area, preferably is selected from hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, percarbonate, Periodic acid, perchloric acid, high boric acid, potassium permanganate and the iron nitrate one or more; What described salt was preferable is sylvite, sodium salt or ammonium salt.What the content of described oxygenant was preferable is mass percent 0.05～10%, and better is mass percent 0.5～5%.
Described complexing agent can be the conventional complexing agent that uses in this area, preferable ammonia carboxylation compound and salt thereof, organic carboxyl acid and salt thereof, one or more in polyamines and organic phospho acid and the salt thereof of being selected from; Described ammonia carboxylation compound is for containing the compound of amino and carboxyl simultaneously, one or more that preferable is in glycine, L-Ala, Xie Ansuan, leucine, proline(Pro), phenylalanine, tyrosine, tryptophane, Methionin, arginine, Histidine, Serine, aspartic acid, L-glutamic acid, l-asparagine, glutamine, nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), hexanaphthene tetraacethyl, diethylene triamine pentacetic acid (DTPA), triethylenetetramine hexaacetic acid and the ethylenediamine disuccinic acid; Described organic carboxyl acid is preferable is in acetic acid, oxalic acid, citric acid, tartrate, propanedioic acid, Succinic Acid, oxysuccinic acid, lactic acid, gallic acid and the sulphosalicylic acid one or more; Described polyamines is preferable is in diethylenetriamine, pentamethyl-diethylenetriamine, triethylene tetramine, tetraethylene pentamine and the polyethylene polyamine one or more; What described organic phospho acid was preferable is 2-phosphonic acids butane-1,2, one or more in 4-tricarboxylic acid, Amino Trimethylene Phosphonic Acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, ethylene diamine tetra methylene phosphonic acid, diethylene triamine pentamethylene phosphonic, polyvalent alcohol phosphonic acid ester, 2-hydroxyethylidene diphosphonic acid guanidine-acetic acid, ethylene diamine tetra methylene phosphonic acid and the polyamino polyether base methylenephosphonic acid.What described salt was preferable is sylvite, sodium salt or ammonium salt.What the content of described complexing agent was preferable is mass percent 0.01～10%, and better is 0.05～5%.
Can also contain the conventional corrosion inhibitor that uses in this area in the polishing fluid of the present invention, it is preferable is in nitrogen azoles, imidazoles, thiazole, pyridine and the pyrimidines one or more; Described nitrogen azole compounds preferably is selected from one or more in following: benzotriazole, 5-methyl isophthalic acid, 2,3-benzotriazole, 5-carboxy benzotriazole, 1-hydroxyl-benzotriazole, 1,2,4-triazole, 3-amino-1,2,4-triazole, 4-amino-1,2,4-triazole, 3, the 5-diaminostilbene, 2,4-triazole, 5-carboxyl-3-amino-1,2,4-triazole, 3-amino-5-sulfydryl-1,2,4-triazole, 5-acetate-1H-tetrazole, 5-methyl tetrazole, 5-amino-1H-tetrazole and 1-phenyl-5-sulfydryl-tetrazole; Described glyoxaline compound preferably is benzoglyoxaline and/or 2-mercaptobenzimidazole; Described thiazole compound preferably is selected from one or more in following: 2-sulfydryl-benzothiazole, 2-dimercaptothiodiazole and 5-amino-2-mercapto phenyl formic-1,3,4-thiadiazoles; Described pyridine compounds and their preferably is one or more in following: 2,3 diamino pyridine, 2-aminopyridine and 2-pyridine carboxylic acid; Described pyrimidines preferably is the 2-aminopyrimidine.What the content of described corrosion inhibitor was preferable is mass percent 0.005～5%, and better is mass percent 0.005～1%.
What described water was preferable is deionized water, and water is supplied content to mass percent 100%.
What the pH of polishing fluid of the present invention was preferable is 2～11, and better is 3～7.
In the polishing fluid of the present invention, can also contain other conventional additives of this area, as pH regulator agent, viscosity modifier, defoamer and sterilant etc.
Polishing fluid of the present invention can prepare as follows: other components except that oxygenant are mixed in proportion, use the conventional pH regulator agent in this area (as KOH, ammoniacal liquor or HNO
3Deng) being adjusted to needed pH value, oxidizer before using mixes and gets final product.
Agents useful for same of the present invention and raw material are all commercially available to be got.
Positive progressive effect of the present invention is: polishing fluid of the present invention can significantly improve the sinking degree of polishing back copper billet, and the chip surface after the polishing not have corrosion under the condition that keeps the higher polishing speed of copper.
Description of drawings
Fig. 1 polishes the back and soaks the back observed surface corrosion situation map of SEM figuratum copper wafer for using embodiment 54 polishing fluids.
Fig. 2 polishes the back and soaks the back observed surface corrosion situation map of SEM with 4 pairs of figuratum copper wafers of comparative example.
Embodiment
Further specify the present invention with embodiment below, but the present invention is not limited.
Table 1 has provided chemical mechanical polishing liquid 1～50 of the present invention, and by the prescription of giving in the table, water is supplied mass percent to 100%, other components except that oxygenant is mixed, with KOH or HNO
3Be adjusted to needed pH value.Oxidizer before using mixes and gets final product.
Table 1 polishing fluid 1～50
Table 2 has provided contrast polishing fluid 1～3 and polishing fluid of the present invention 51～53, by the prescription of giving in the table, other components except that oxygenant is mixed, and water is supplied mass percent to 100%, with KOH or HNO
3Be adjusted to needed pH value.Oxidizer before using mixes and gets final product.
Table 2 contrast polishing fluid 1 and polishing fluid 51～53
Adopt contrast polishing fluid 1～3 and 51～53 pairs of empty sheet copper of polishing fluid of the present invention (Cu) wafer to polish, remove speed and see Table 3.
Polishing material: empty sheet copper wafer; Polishing condition: overdraft 3Psi, polishing disk and rubbing head rotating speed 70/80rpm, polishing pad PPG MX710, polishing fluid flow velocity 100ml/min, polishing machine platform are LogitechPM5 Polisher.
Table 3 contrast polishing fluid 1～3 and 51～53 pairs of metallic coppers of polishing fluid are removed speed
| Polishing fluid | The removal speed (A/min) of |
| Contrast | |
| 1 | ??8865 |
| Contrast 2 | ??10251 |
| Contrast 3 | ??14824 |
| ??51 | ??4316 |
| ??52 | ??3859 |
| ??53 | ??8537 |
By table as seen, compare with the comparative example 1～3 of block polyether, added the block polyether of different concns in the polishing fluid 51～53, this block polyether can effectively suppress the removal speed of copper.
Effect embodiment 2
Table 4 has provided contrast polishing fluid 4 and polishing fluid of the present invention 54, by the prescription of giving in the table, other components except that oxygenant is mixed, and water is supplied mass percent to 100%, with KOH or HNO
3Be adjusted to needed pH value.Oxidizer before using mixes and gets final product.
Table 4 contrast polishing fluid 4 and polishing fluid of the present invention 54
Adopt contrast polishing fluid 4 and polishing fluid 54, empty sheet copper (Cu), tantalum (Ta), silicon-dioxide (Teos) wafer and figuratum copper wafer are polished, see Table 5.
Empty sheet polishing condition: copper wafer: overdraft 3Psi/1psi; Tantalum (Ta) and silicon-dioxide (Teos) wafer: overdraft 1psi, polishing disk and rubbing head rotating speed 70/80rpm, polishing pad PPG MX710, polishing fluid flow velocity 100ml/min, polishing machine platform are Logitech PM5Polisher.
Figuratum copper wafer polishing processing condition: overdraft 3psi polishes figuratum copper wafer to the about 2000A of remaining copper, and then under 1psi residual copper is removed and crossed and threw 30 seconds.Measure the depression value of the copper billet of 80um*80um on the figuratum copper wafer with the XE-300P atomic force microscope.Polishing disk and rubbing head rotating speed 70/80rpm, polishing pad PPG MX710, polishing fluid flow velocity 100ml/min, polishing machine platform are Logitech PM5 Polisher.
Table 5
See by table 5, compare with the comparative example 4 of block polyether not, added block polyether among the embodiment 54, the removal speed of inhibition copper under low overdraft that this block polyether energy is more, help being reduced in the depression on the figuratum copper wafer, and under high pressure, can keep higher copper to remove speed, thereby do not influence throughput.
Effect embodiment 3
Adopt the polishing fluid of comparative example 4 and embodiment 54, figuratum copper wafer is polished and soaks.
Polishing technological conditions: polishing disk and rubbing head rotating speed 70/80rpm, polishing pad PPG MX710, polishing fluid flow velocity 100ml/min, polishing machine platform are Logitech PM5 Polisher.Overdraft 3psi polishes figuratum copper wafer to the about 2000A of remaining copper, and then 1psi removes residual copper and cross and threw 30 seconds down.Copper wafer after the polishing was immersed in the polishing fluid after 30 minutes, takes out wafer surface is observed in the back with scanning electronic microscope (SEM) the corrosion situation of cleaning.
Show that by Fig. 1 in the polishing and the figuratum copper wafer after the immersion with polishing fluid of the present invention, copper line surface and edge do not have corrosion.And with in the copper wafer (see figure 2) after comparative example's 4 polishings, there is obvious corrosion phenomenon at copper line surface and edge.
Claims (17)
1. chemical mechanical polishing liquid, it contains abrasive grains, complexing agent, oxygenant and water, it is characterized in that: described chemical mechanical polishing liquid also contains one or more block polyether class tensio-active agents.
2. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: described block polyether class tensio-active agent is polyoxyethylene-poly-oxypropylene polyoxyethylene three block polyethers, and it is represented with formula I, (CH
2CH
2O)
x-(CH (CH
3) CH
2O)
y-(CH
2CH
2O)
z-OH is designated as (EO)
x(PO)
y(EO)
z
Formula I
Wherein, 10≤x, y, z≤150.
3. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the content of described block polyether class tensio-active agent is mass percent 0.001～3%.
4. chemical mechanical polishing liquid as claimed in claim 3 is characterized in that: the content of described block polyether class tensio-active agent is mass percent 0.001～1%.
5. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: described oxygenant is one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, percarbonate, Periodic acid, perchloric acid, high boric acid, potassium permanganate and the iron nitrate.
6. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the content of described oxygenant is mass percent 0.05～10%.
7. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: described complexing agent is one or more in the following compound: ammonia carboxylation compound and salt thereof, organic carboxyl acid and salt thereof, polyamines and organic phospho acid and salt thereof.
8. chemical mechanical polishing liquid as claimed in claim 7 is characterized in that: described ammonia carboxylation compound is one or more in glycine, L-Ala, Xie Ansuan, leucine, proline(Pro), phenylalanine, tyrosine, tryptophane, Methionin, arginine, Histidine, Serine, aspartic acid, L-glutamic acid, l-asparagine, glutamine, nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), hexanaphthene tetraacethyl, ethylenediamine disuccinic acid, diethylene triamine pentacetic acid (DTPA) and the triethylenetetramine hexaacetic acid; Described organic carboxyl acid is one or more in acetic acid, oxalic acid, citric acid, tartrate, propanedioic acid, Succinic Acid, oxysuccinic acid, lactic acid, gallic acid and the sulphosalicylic acid; Described polyamines is one or more in diethylenetriamine, pentamethyl-diethylenetriamine, triethylene tetramine, tetraethylene pentamine and the polyethylene polyamine; Described organic phospho acid is a 2-phosphonic acids butane-1,2, one or more in 4-tricarboxylic acid, Amino Trimethylene Phosphonic Acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, ethylene diamine tetra methylene phosphonic acid, diethylene triamine pentamethylene phosphonic, polyvalent alcohol phosphonic acid ester, 2-hydroxyethylidene diphosphonic acid guanidine-acetic acid, ethylene diamine tetra methylene phosphonic acid and the polyamino polyether base methylenephosphonic acid; Described salt is sylvite, sodium salt or ammonium salt.
9. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the content of described complexing agent is mass percent 0.01～10%.
10. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: described abrasive grains is one or more in silicon-dioxide, cerium dioxide, titanium dioxide and the polymer abrasive grains of silicon-dioxide, aluminium coating of silicon-dioxide, aluminum oxide, adulterated al.
11. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the content of described abrasive grains is mass percent 0.1～5%.
12. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the particle diameter of described abrasive grains is 20～150nm.
13. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: described chemical mechanical polishing liquid also contains corrosion inhibitor.
14. chemical mechanical polishing liquid as claimed in claim 13 is characterized in that: described corrosion inhibitor is one or more in nitrogen azoles, imidazoles, thiazole, pyridine and the pyrimidines.
15. chemical mechanical polishing liquid as claimed in claim 14, it is characterized in that: described nitrogen azole compounds is selected from one or more in following: benzotriazole, the 5-methyl isophthalic acid, 2, the 3-benzotriazole, the 5-carboxy benzotriazole, 1-hydroxyl-benzotriazole, 1,2, the 4-triazole, 3-amino-1,2, the 4-triazole, 4-amino-1,2, the 4-triazole, 3, the 5-diaminostilbene, 2, the 4-triazole, 5-carboxyl-3-amino-1,2, the 4-triazole, 3-amino-5-sulfydryl-1,2, the 4-triazole, 5-acetate-1H-tetrazole, 5-methyl tetrazole, 5-amino-1H-tetrazole and 1-phenyl-5-sulfydryl-tetrazole; Described glyoxaline compound is benzoglyoxaline and/or 2-mercaptobenzimidazole; Described thiazole compound is selected from one or more in following: 2-sulfydryl-benzothiazole, 2-dimercaptothiodiazole and 5-amino-2-mercapto phenyl formic-1,3,4-thiadiazoles; Described pyridine compounds and their is selected from one or more in following: 2,3 diamino pyridine, 2-aminopyridine and 2-pyridine carboxylic acid; Described pyrimidines is the 2-aminopyrimidine.
16. chemically machinery polished as claimed in claim 13 is characterized in that: the content of described corrosion inhibitor is mass percent 0.005～5%.
17. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the pH of described polishing fluid is 2～11.
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|---|---|---|---|
| CN200810207473A CN101747843A (en) | 2008-12-19 | 2008-12-19 | Chemical-mechanical polishing solution |
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|---|---|---|---|
| CN200810207473A CN101747843A (en) | 2008-12-19 | 2008-12-19 | Chemical-mechanical polishing solution |
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