CN101665664A - Quaternary ammonium salt cationic surfactant and application of chemical mechanical polishing solution - Google Patents
Quaternary ammonium salt cationic surfactant and application of chemical mechanical polishing solution Download PDFInfo
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- CN101665664A CN101665664A CN200810042571A CN200810042571A CN101665664A CN 101665664 A CN101665664 A CN 101665664A CN 200810042571 A CN200810042571 A CN 200810042571A CN 200810042571 A CN200810042571 A CN 200810042571A CN 101665664 A CN101665664 A CN 101665664A
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Abstract
The invention discloses application of a quaternary ammonium salt cationic surfactant in preparing chemical mechanical polishing solution for a low dielectric material, and also discloses applicationof the chemical mechanical polishing solution in polishing the low dielectric material. The chemical mechanical polishing solution comprises polishing particles, the quaternary ammonium salt cationicsurfactant, a corrosion inhibitor, a complexing agent, an oxidant and water. In the application, the quaternary ammonium salt cationic surfactant and the polishing solution containing the same can inhibit the polishing velocity of the low dielectric material (such as BD), but do not have great influence on the velocity of removing copper, tantalum and silicon dioxide (Teos).
Description
Technical field
The present invention relates to the new application of quaternary ammonium salt cationic surfactant and a kind of chemical mechanical polishing liquid.
Background technology
Tradition dielectric layer material (as TEOS) is owing to have higher dielectric constant, can cause electric capacity increase between the conducting stratum, thereby influence the speed of unicircuit, efficient is reduced, along with the complicated of unicircuit and becoming more meticulous, this base material can not satisfy more (65nm or 45nm) technical requirements of advanced process all the more, and introducing dielectric materials (as CDO, SOG) in substrate is the inexorable trend of integrated circuit technique development, has produced many polishing slurries that are used for dielectric materials thereupon.
But present low-dielectric material lapping liquid of the prior art does not all reach the perfect adaptation of manufacturing cost and technology performance.Disclose a kind of acid slurry as patent documentation US6046112, adopted ZrO
2Be abrasive material, cooperate azanol, come polishing low dielectric material SOG.The abrasive material price height that is adopted, the production cost height.Patent documentation US6974777 discloses a kind of polishing fluid that is used for dielectric materials for another example, this polishing fluid includes a kind of HLB value greater than 7 nonionogenic tenside, this nonionogenic tenside can suppress the polishing speed of dielectric materials, and little to the removal speed influence of copper and tantalum.
Summary of the invention
Technical problem to be solved by this invention provides the application of quaternary ammonium salt cationic surfactant in the chemical mechanical polishing liquid of preparation dielectric materials.The present invention finds that after deliberation quaternary ammonium salt cationic surfactant can suppress the polishing speed of dielectric materials (as BD), and little to the removal speed influence of copper, tantalum and silicon-dioxide (Teos).
Preferable, the invention provides a kind of chemical mechanical polishing liquid of quaternary ammonium salt cationic surfactant that contains in the application in polishing low dielectric material.Described chemical mechanical polishing liquid comprises abrasive grains, quaternary ammonium salt cationic surfactant, corrosion inhibitor, complexing agent, oxygenant and water.
Among the present invention, what described quaternary ammonium salt cationic surfactant was preferable is mono-quaternaries type cats product and/or double type quaternary cationics.
That wherein, described mono-quaternaries type cats product is preferable is R
1R
2N
+R
3R
4X
-, wherein: R
1For-C
mH
2m+1, 8≤m≤22; R
2And R
3Identical, for-CH
3Or-C
2H
5R
4With R
1Identical, or R
4For-CH
3,-C
2H
5,-CH
2-C
6H
5Or-CH
2CH
2OH; X
-Be Cl
-, Br
-, CH
3SO
4 -, NO
3 -Or C
6H
5-SO
4 -
That wherein, described double type quaternary cationics is preferable is (R
1R
2N
+R
3X
-)-R
5-(R
1' R
2N
+R
3X
-), wherein: R
1And R
1' be-C
mH
2m+1, 8≤m≤18, R
1And R
1' identical or different; R
2And R
3Identical, for-CH
3Or-C
2H
5R
5Be phenylenedimethylidyne, polymethylene-(CH
2)
n-, 2≤n≤30, or polyoxyethylene groups-CH
2CH
2-(OCH
2CH
2)
n-, 1≤n≤30; X
-Be Cl
-Or Br
-
What the weight percent concentration of described quaternary ammonium salt cationic surfactant in chemical mechanical polishing liquid was preferable is 0.0001～1%, and better is 0.001～0.5%.
Among the present invention, described abrasive grains can be this area abrasive grains commonly used, as the silicon-dioxide of the silicon-dioxide of silicon-dioxide, aluminium sesquioxide, cerium dioxide, titanium dioxide, aluminium coating, adulterated al and/or polymer beads etc.What the weight percent concentration of abrasive grains was preferable is 1～20%, and better is 2～10%.That the particle diameter of described abrasive grains is preferable is 20～150nm, and that better is 30～120nm.
Among the present invention, described corrosion inhibitor can be this area corrosion inhibitor commonly used, preferable be selected from following one or more: benzotriazole, 1,2,4-triazole, 3-amino-1,2,4-triazole, 4-amino-1,2,4-triazole, 5-carboxyl-3-amino-1,2,4-triazole, 5-acetate-1H-tetrazole, 5-methyl tetrazole, 5-amino-1H-tetrazole, 1-phenyl-5-sulfydryl-tetrazole, 2-sulfydryl-benzothiazole, benzoglyoxaline and 2-mercaptobenzimidazole.What the weight percent concentration of corrosion inhibitor was preferable is 0.001～2%, and better is 0.01～1%.
Among the present invention, described complexing agent can be this area complexing agent commonly used, preferable is selected from following one or more: inorganic phosphate and salt thereof and organic phosphoric acid and salt thereof.Wherein, what described inorganic phosphate and salt thereof were preferable is phosphoric acid, phosphorous acid, tetra-sodium, three metaphosphoric acids, hexa metaphosphoric acid, tripolyphosphate, polyphosphoric acid, and the salt of above-mentioned acid; What described organic phosphoric acid and salt thereof were preferable is 2-phosphonic acids butane group-1; 2; 4-tricarboxylic acid, ethylenediamine tetramethylene phosphonic acid, diethylene triamine pentamethylene phosphonic, hydroxy ethylene diphosphonic acid, Amino Trimethylene Phosphonic Acid, 2-HPAA, polyamino polyether methylene phosphonic acids, and the salt of above-mentioned acid.What described salt was preferable is sodium salt, sylvite or ammonium salt.What the weight percent concentration of complexing agent was preferable is 0.001～2%, and better is 0.01～1%.
Among the present invention, described oxygenant can be this area oxygenant commonly used, preferable is selected from following one or more: hydrogen peroxide, urea peroxide, Peracetic Acid, Potassium Persulphate and ammonium persulphate.What the weight percent concentration of oxygenant was preferable is 0.001～5%, and better is 0.05～2%.
Among the present invention, the consumption of described water is for supplying weight percent 100%.
Among the present invention, what the pH value of described chemical mechanical polishing liquid was preferable is 2.0～7.0, and better is 2.0～5.0.
Among the present invention, described chemical mechanical polishing liquid also can comprise anion surfactant.Use anion surfactant can reduce the surface contaminant of polished material.The preferred anionic surfactants tensio-active agent is polycarboxylic acid compound and/or its salt.Described polycarboxylic acid compound is preferable be polyacrylic acid and with maleic anhydride, acrylate and cinnamic multipolymer in one or more, what described salt was preferable is ammonium salt, sylvite or sodium salt; What the molecular weight of described polycarboxylic acid compound or its salt was preferable is 2,000～100,000.What the weight percent concentration of anion surfactant was preferable is 0.0001～1%, and better is 0.001～0.5%.
Among the present invention, described chemical mechanical polishing liquid can also comprise other this area conventional additives such as pH regulator agent, viscosity modifier and sterilant.
Polishing fluid of the present invention can prepare as follows: other components except that oxygenant are mixed in proportion, use the pH regulator agent (as KOH or HNO
3) 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: quaternary ammonium salt cationic surfactant, and the chemical mechanical polishing liquid that contains it of the present invention can suppress the polishing speed of dielectric materials (as BD), and little to the removal speed influence of copper, tantalum and silicon-dioxide.
Embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.
Embodiment 1～22
Table 1 has provided the chemical mechanical polishing liquid embodiment 1～20 that is applied to the dielectric materials polishing, by the prescription of giving in the table, 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.Water is supplied mass percent 100%.
Table 1 blocking layer chemical mechanical polishing liquid embodiment 1～22
Embodiment 23～35
Embodiment 23～35 all contains 10wt% silicon-dioxide (70nm), 0.1wt% benzotriazole, 0.01wt% phosphoric acid, the 1wt% hydrogen peroxide, with 0.001wt% diethoxy-two (dodecyl dimethyl brometo de amonios), also contain polycarboxylic acid compound and/or its salt respectively, as shown in table 2.The preparation method is the same.
Table 2 embodiment 23～35 contained polycarboxylic acid compound and pH thereof
| Embodiment | Content wt% | Anion surfactant | ??pH |
| ??23 | ??1 | Polyacrylic acid (molecular weight 2000) | ??3 |
| ??24 | ??0.5 | Polyacrylic acid potassium (molecular weight 5000) | ??4 |
| ??25 | ??0.001 | Sodium polyacrylate (molecular weight 10000) | ??5 |
| ??26 | ??0.0001 | Ammonium polyacrylate (molecular weight 100000) | ??3 |
| ??27 | ??1 | Vinylformic acid copolymer-maleic anhydride (molecular weight 2000) | ??3 |
| ??28 | ??0.01 | Vinylformic acid copolymer-maleic anhydride sylvite (molecular weight 100000) | ??3 |
| ??29 | ??0.05 | Vinylformic acid copolymer-maleic anhydride ammonium salt (molecular weight 20000) | ??3 |
| ??30 | ??0.5 | Vinylformic acid styrol copolymer (molecular weight 2000) | ??3 |
| ??31 | ??0.001 | Vinylformic acid styrol copolymer ammonium salt (molecular weight 100000) | ??3 |
| ??32 | ??0.02 | Vinylformic acid styrol copolymer sodium salt (molecular weight 10000) | ??3 |
| ??33 | ??0.8 | Acrylic acrylate multipolymer (molecular weight 2000) | ??3 |
| ??34 | ??0.005 | Acrylic acrylate multipolymer ammonium salt (molecular weight 100000) | ??3 |
| ??35 | ??0.03 | Acrylic acrylate multipolymer sylvite (molecular weight 50000) | ??3 |
Effect embodiment 1
Table 3 has provided contrast polishing fluid 1 and polishing fluid of the present invention 1～5, by the prescription of giving in the table, 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.Water supplies 100%.
Table 3 contrast polishing fluid 1 and polishing fluid of the present invention 1～5
Adopt contrast polishing fluid 1 and 1～5 pair of copper of polishing fluid of the present invention, tantalum, silicon-dioxide (Teos) and dielectric materials (BD) wafer to polish, remove speed and see Table 4.
Polishing material: copper, tantalum, silicon-dioxide (Teos) wafer and dielectric materials (BD); Polishing condition: 2Psi, polishing disk and rubbing head rotating speed 70/80rpm, polishing pad Politex, polishing fluid flow velocity 100ml/min, Logitech PM5 Polisher.
Table 4 contrast polishing fluid 1 and polishing fluid of the present invention 1～5
Removal speed to metallic copper (Cu), silicon-dioxide (Teos) and metal smooth (Ta)
By table as seen, compare with the comparative example 1 who does not add any quaternary ammonium salt, the removal speed influence of polishing fluid 1～5 pair of copper, tantalum and silicon-dioxide (Teos) of quaternary ammonium salt of having added different concns among the effect embodiment 1 is little, and the removal speed of dielectric materials BD is suppressed bigger.
Effect embodiment 2
Adopt the polishing fluid of embodiment 24, and the polishing fluid of addition polymerization carboxylic acid compound and/or its salt not, be 10wt% silicon-dioxide (70nm), the 0.1wt% benzotriazole, 0.01wt% phosphoric acid, 1wt% hydrogen peroxide and 0.001wt% diethoxy-two (dodecyl dimethyl brometo de amonios) polish figuratum copper wafer, and polishing technological conditions is the same.
After the polishing, the surface imperfection of polishing on back 8 inches copper wafers with the polishing fluid of embodiment 24 adds up to 114, and the surface imperfection sum that adopts the polishing fluid of addition polymerization carboxylic acid compound not and/or its salt to polish on back 8 inches copper wafers reaches 2150.Employed detecting instrument is KLA-Tenkorbright field inspector.
By above-mentioned description of test, after polishing fluid of the present invention adds anion surfactant, can significantly reduce the surface contaminant of polished material.
Claims (28)
1, the application of quaternary ammonium salt cationic surfactant in the chemical mechanical polishing liquid of preparation dielectric materials.
2, the application of a kind of chemical mechanical polishing liquid in polishing low dielectric material is characterized in that: described chemical mechanical polishing liquid contains abrasive grains, quaternary ammonium salt cationic surfactant, corrosion inhibitor, complexing agent, oxygenant and water.
3, application according to claim 1 and 2 is characterized in that: described quaternary ammonium salt cationic surfactant is mono-quaternaries type cats product and/or double type quaternary cationics.
4, application according to claim 3 is characterized in that:
Described mono-quaternaries type cats product is R
1R
2N
+R
3R
4X
-, wherein: R
1For-C
mH
2m+1, 8≤m≤22; R
2And R
3Identical, for-CH
3Or-C
2H
5R
4With R
1Identical, or R
4For-CH
3,-C
2H
5,-CH
2-C
6H
5Or-CH
2CH
2OH; X
-Be Cl
-, Br
-, SO
4 -, CH
3SO
4 -, NO
3 -Or C
6H
5-SO
4 -
Described double type quaternary cationics is (R
1R
2N
+R
3X
-)-R
5-(R
1' R
2N
+R
3X
-), wherein: R
1And R
1' be-C
mH
2m+1, 8≤m≤18, R
1And R
1' identical or different; R
2And R
3Identical, for-CH
3Or-C
2H
5R
5Be phenylenedimethylidyne, polymethylene-(CH
2)
n-, 2≤n≤30, or polyoxyethylene groups-CH
2CH
2-(OCH
2CH
2)
n-, 1≤n≤30; X
-Be Cl
-Or Br
-
5, application according to claim 1 and 2 is characterized in that: the weight percent concentration of described quaternary ammonium salt cationic surfactant is 0.0001～1%.
6, application according to claim 5 is characterized in that: the weight percent concentration of described quaternary ammonium salt cationic surfactant is 0.001～0.5%.
7, application according to claim 2 is characterized in that: described abrasive grains is the silicon-dioxide of silicon-dioxide, aluminium sesquioxide, cerium dioxide, titanium dioxide, aluminium coating, the silicon-dioxide and/or the polymer beads of adulterated al.
8, application according to claim 2 is characterized in that: the weight percent concentration of described abrasive grains is 1～20%.
9, application according to claim 8 is characterized in that: the weight percent concentration of described abrasive grains is 2～10%.
10, application according to claim 2 is characterized in that: described corrosion inhibitor is an azole compounds.
11, application according to claim 10 is characterized in that: described azole compounds is one or more in nitrogen azoles, thiazole and the imidazoles.
12, application according to claim 10, it is characterized in that: described azole compounds is selected from one or more in following: benzotriazole, 1,2,4-triazole, 3-amino-1,2,4-triazole, 4-amino-1,2,4-triazole, 5-carboxyl-3-amino-1,2,4-triazole, 5-acetate-1H-tetrazole, 5-methyl tetrazole, 5-amino-1H-tetrazole, 1-phenyl-5-sulfydryl-tetrazole, 2-sulfydryl-benzothiazole, benzoglyoxaline and 2-mercaptobenzimidazole.
13, application according to claim 2 is characterized in that: the weight percent concentration of described corrosion inhibitor is 0.001～2%.
14, application according to claim 13 is characterized in that: the weight percent concentration of described corrosion inhibitor is 0.01～1%.
15, application according to claim 2 is characterized in that: described complexing agent is selected from one or more in following: inorganic phosphate and salt thereof and organic phosphoric acid and salt thereof.
16, application according to claim 15 is characterized in that:
Described inorganic phosphate and salt thereof are phosphoric acid, phosphorous acid, tetra-sodium, three metaphosphoric acids, hexa metaphosphoric acid, tripolyphosphate, polyphosphoric acid, and the salt of above-mentioned acid;
Described organic phosphoric acid and salt thereof are 2-phosphonic acids butane group-1,2,4-tricarboxylic acid, ethylenediamine tetramethylene phosphonic acid, diethylene triamine pentamethylene phosphonic, hydroxy ethylene diphosphonic acid, Amino Trimethylene Phosphonic Acid, 2-HPAA, polyamino polyether methylene phosphonic acids, and the salt of above-mentioned acid;
Described salt is ammonium salt, sylvite or sodium salt.
17, application according to claim 2 is characterized in that: the weight percent concentration of described complexing agent is 0.001～2%.
18, application according to claim 17 is characterized in that: the weight percent concentration of described complexing agent is 0.01～1%.
19, application according to claim 2 is characterized in that: described oxygenant is selected from one or more in following: hydrogen peroxide, urea peroxide, Peracetic Acid, Potassium Persulphate and ammonium persulphate.
20, application according to claim 2 is characterized in that: the weight percent concentration of described oxygenant is 0.001～5%.
21, application according to claim 20 is characterized in that: the weight percent concentration of described oxygenant is 0.05～2%.
22, application according to claim 2 is characterized in that: the pH value of described polishing fluid is 2.0～7.0.
23, application according to claim 22 is characterized in that: the pH value of described polishing fluid is 2.0～5.0.
24, application according to claim 2 is characterized in that: described polishing fluid also comprises anion surfactant.
25, application according to claim 24 is characterized in that: described anion surfactant is one or more in polycarboxylic acid compound and the salt thereof.
26, application according to claim 25 is characterized in that: described polycarboxylic acid compound be polyacrylic acid and with maleic anhydride, acrylate and cinnamic multipolymer in one or more; Described salt is ammonium salt, sylvite or sodium salt; Molecular weight is 2,000～100,000.
27, application as claimed in claim 22 is characterized in that: the weight percent concentration of described anion surfactant is 0.0001～1%.
28, application as claimed in claim 27 is characterized in that: the weight percent concentration of described anion surfactant is 0.001～0.5%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011069344A1 (en) * | 2009-12-11 | 2011-06-16 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing liquid |
| CN102464947A (en) * | 2010-11-19 | 2012-05-23 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| CN102559354A (en) * | 2010-12-30 | 2012-07-11 | 安集微电子（上海）有限公司 | Water-based glass grinding fluid |
| CN103184009A (en) * | 2011-12-27 | 2013-07-03 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid |
| CN103834306A (en) * | 2012-11-22 | 2014-06-04 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid for through-silicon-via planarization |
| CN103894918A (en) * | 2012-12-28 | 2014-07-02 | 安集微电子（上海）有限公司 | Chemical mechanical polishing method |
| CN103184009B (en) * | 2011-12-27 | 2016-12-14 | 安集微电子（上海）有限公司 | A kind of chemical mechanical polishing liquid |
| WO2017074800A1 (en) * | 2015-10-28 | 2017-05-04 | Cabot Microelectronics Corporation | Tungsten-processing slurry with cationic surfactant and cyclodextrin |
| CN114958206A (en) * | 2021-02-22 | 2022-08-30 | 万华化学集团电子材料有限公司 | Copper chemical mechanical polishing solution, application thereof and chemical mechanical polishing method |
| WO2023098719A1 (en) * | 2021-11-30 | 2023-06-08 | 安集微电子（上海）有限公司 | Method for preparing cerium oxide nanocomposite, cerium oxide nanocomposite, and chemical mechanical polishing solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011069344A1 (en) * | 2009-12-11 | 2011-06-16 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing liquid |
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| CN102559354A (en) * | 2010-12-30 | 2012-07-11 | 安集微电子（上海）有限公司 | Water-based glass grinding fluid |
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| CN103184009B (en) * | 2011-12-27 | 2016-12-14 | 安集微电子（上海）有限公司 | A kind of chemical mechanical polishing liquid |
| CN103834306A (en) * | 2012-11-22 | 2014-06-04 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid for through-silicon-via planarization |
| CN103834306B (en) * | 2012-11-22 | 2017-08-11 | 安集微电子（上海）有限公司 | A kind of chemical mechanical polishing liquid planarized for silicon hole |
| CN103894918A (en) * | 2012-12-28 | 2014-07-02 | 安集微电子（上海）有限公司 | Chemical mechanical polishing method |
| WO2017074800A1 (en) * | 2015-10-28 | 2017-05-04 | Cabot Microelectronics Corporation | Tungsten-processing slurry with cationic surfactant and cyclodextrin |
| CN114958206A (en) * | 2021-02-22 | 2022-08-30 | 万华化学集团电子材料有限公司 | Copper chemical mechanical polishing solution, application thereof and chemical mechanical polishing method |
| CN114958206B (en) * | 2021-02-22 | 2024-02-02 | 万华化学集团电子材料有限公司 | Copper chemical mechanical polishing solution and application thereof and chemical mechanical polishing method |
| WO2023098719A1 (en) * | 2021-11-30 | 2023-06-08 | 安集微电子（上海）有限公司 | Method for preparing cerium oxide nanocomposite, cerium oxide nanocomposite, and chemical mechanical polishing solution |
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