CN115725239B - Preparation method of faint scent type polishing solution composition - Google Patents
Preparation method of faint scent type polishing solution composition Download PDFInfo
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- CN115725239B CN115725239B CN202211442202.2A CN202211442202A CN115725239B CN 115725239 B CN115725239 B CN 115725239B CN 202211442202 A CN202211442202 A CN 202211442202A CN 115725239 B CN115725239 B CN 115725239B
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- 238000005498 polishing Methods 0.000 title claims abstract description 123
- 239000000203 mixture Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- BJRNKVDFDLYUGJ-RMPHRYRLSA-N hydroquinone O-beta-D-glucopyranoside Chemical group O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C(O)C=C1 BJRNKVDFDLYUGJ-RMPHRYRLSA-N 0.000 claims abstract description 34
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 15
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 6
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 claims description 4
- VHLJDTBGULNCGF-UHFFFAOYSA-N Limonin Natural products CC1(C)OC2CC(=O)OCC23C4CCC5(C)C(CC(=O)C6OC56C4(C)C(=O)CC13)c7cocc7 VHLJDTBGULNCGF-UHFFFAOYSA-N 0.000 claims description 3
- KBDSLGBFQAGHBE-MSGMIQHVSA-N limonin Chemical compound C=1([C@H]2[C@]3(C)CC[C@H]4[C@@]([C@@]53O[C@@H]5C(=O)O2)(C)C(=O)C[C@@H]2[C@]34COC(=O)C[C@@H]3OC2(C)C)C=COC=1 KBDSLGBFQAGHBE-MSGMIQHVSA-N 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 229940087305 limonene Drugs 0.000 claims description 2
- 235000001510 limonene Nutrition 0.000 claims description 2
- 239000008139 complexing agent Substances 0.000 abstract description 26
- 239000004094 surface-active agent Substances 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 12
- 235000005979 Citrus limon Nutrition 0.000 abstract description 10
- 230000003746 surface roughness Effects 0.000 abstract description 4
- 244000248349 Citrus limon Species 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 24
- 230000009471 action Effects 0.000 description 16
- 239000007788 liquid Substances 0.000 description 13
- 238000007517 polishing process Methods 0.000 description 11
- 244000131522 Citrus pyriformis Species 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 229960000271 arbutin Drugs 0.000 description 6
- BJRNKVDFDLYUGJ-UHFFFAOYSA-N p-hydroxyphenyl beta-D-alloside Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(O)C=C1 BJRNKVDFDLYUGJ-UHFFFAOYSA-N 0.000 description 6
- 229910052594 sapphire Inorganic materials 0.000 description 6
- 239000010980 sapphire Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000536 complexating effect Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
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- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 244000302512 Momordica charantia Species 0.000 description 1
- 235000009811 Momordica charantia Nutrition 0.000 description 1
- 235000009812 Momordica cochinchinensis Nutrition 0.000 description 1
- 235000018365 Momordica dioica Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 244000137773 Viola philippica Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- -1 aluminate ions Chemical class 0.000 description 1
- 239000002519 antifouling agent Substances 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229920002674 hyaluronan Polymers 0.000 description 1
- 229960003160 hyaluronic acid Drugs 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
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- 239000003112 inhibitor Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention provides a preparation method of a fragrant polishing solution composition, which comprises a silica sol grinding medium, a complexing agent, a surfactant, a pH regulator, essence and deionized water, wherein the complexing agent is selected from p-hydroxyphenyl-beta-D-glucopyranoside, the polishing solution has higher material removal rate and lower surface roughness, the obtained polishing material has smooth surface, no scratch, low surface polishing medium residue rate and convenient post-polishing treatment, and the polishing solution composition has lemon smell.
Description
Technical Field
The invention relates to the technical field of preparation of polishing materials, in particular to polishing solution for an alumina wafer substrate.
Background
The chemical mechanical polishing (Chemical Mechanical Polishing, abbreviated as CMP) technology can give consideration to the global and local flatness of the processed surface, is a truly atomic molecular-level limit processing technology, and is one of core technologies in the field of semiconductor manufacturing.
The chemical mechanical polishing technology organically combines chemical action and mechanical action, and finishes polishing of the surface of the monocrystalline sapphire wafer in the alternate process of the two actions, so that the polishing mode can effectively avoid the defects of surface damage caused by simple mechanical polishing, low polishing speed, poor surface flatness and polishing consistency and the like which are easy to cause by simple chemical polishing. The rate controlling factor of the entire polishing process is the slower of the two: when the mechanical action is greater than the chemical action, the surface processing stress is increased, and surface defects such as scratches and the like are extremely easy to form on the processing surface at the moment, so that a high damage layer is generated; when the chemical action is large and the mechanical action is performed, the selectivity of material removal is reduced, and orange peel and corrosion pits are easily formed on the processing surface. Chemical mechanical polishing requires that the chemical and mechanical actions be as balanced as possible, i.e., that the chemical removal rate be equal to the mechanical removal rate.
The polishing solution plays a very important role in the chemical mechanical polishing process: firstly, chemical components in the polishing solution react with the surface of a wafer to form a layer of thin oxide film with weak binding force on the processing surface of a workpiece, and then abrasive particles in the polishing solution are used for trace removal of the surface of the workpiece under the action of pressure and friction, and the two processes are continuously carried out under the action of the polishing solution, so that the polishing of the surface of the wafer is completed.
The chemical mechanical polishing solution comprises the basic components of abrasive, pH value regulator, oxidant, dispersant and deionized water. The grain size, hardness, and shape of the abrasive often determine the thickness of the mechanically removed surface material during chemical mechanical polishing. The most desirable abrasive is one whose thickness of the removed surface material is comparable to the thickness of the chemically oxidized film, in which case the damage to the wafer surface from chemical mechanical polishing is minimized.
A great deal of scholars have conducted intensive studies on the abrasive components in the chemical mechanical polishing liquid, but the following problems exist in the prior art: the components of the polishing solution are complex, and particularly, a large amount of accelerator, corrosion inhibitor or other metal salts are introduced, so that the post-polishing treatment is difficult, and the residual rate of the polishing solution on the surface of the wafer is too high; in addition, the selectivity of the complexing agent is low, the removal rate of the obtained material is reduced, and the high-precision polishing effect cannot be effectively obtained.
Disclosure of Invention
Based on the technical problems existing in the prior art, the invention provides a preparation method of a faint scent type polishing solution composition, which has excellent removal rate and lower roughness for polishing an alumina wafer, the obtained polishing material has smooth surface, no scratch, low surface polishing medium residue rate and convenient post-polishing treatment, and the main reasons are due to the fact that p-hydroxyphenyl-beta-D-glucopyranoside is introduced into the polishing solution for the first time as a complexing agent for selecting, and the preparation method comprises the following steps:
a preparation method of a faint scent type polishing solution composition comprises the following steps:
(1) Dispersing silica sol grinding medium with particle size of 20-30nm in proper amount of deionized water, adding hydroxyethyl ethylenediamine surfactant while stirring, stirring at 100-150rpm for 10-15min at normal temperature to form stable suspension;
(2) Adding p-hydroxyphenyl-beta-D-glucopyranoside complexing agent into the suspension solution, stirring at the speed of 100-150rpm at the temperature of 30-35 ℃ for 2-3min, and supplementing the rest normal-temperature deionized water containing limonin;
(3) Adjusting the pH value of the solution to be within the range of 10-11 by using a diethylenetriamine pH regulator to obtain the wafer faint scent type polishing solution composition;
the fragrant polishing solution composition comprises the following components in percentage by mass:
10-25 wt% of silica sol grinding medium: the size of the silicon oxide abrasive medium particles is concentrated at 20-30nm, and D98 is less than or equal to 40nm;
2.5-2.8wt.% complexing agent: p-hydroxyphenyl-beta-D-glucopyranoside;
0.5 to 0.7wt.% surfactant: hydroxyethyl ethylenediamine;
0.01-0.05wt.% limonene essence;
pH regulator: diethylenetriamine, and adjusting the pH value to be in the range of 10-11;
and the balance of deionized water.
The faint scent type polishing solution composition is obtained by a preparation method of the faint scent type polishing solution composition, and the polishing roughness Ra=0.4-0.6 nm of an aluminum oxide wafer obtained by treatment of the faint scent type polishing solution composition has a removal rate of 1.67-1.94 mu m/h. Further, after polishing, the alumina wafer is put into an ultrasonic cleaner with 60W and 40KHz for 2-3min, the solution in the ultrasonic cleaner is 50wt.% ethanol solution, and then the alumina wafer is dried, wherein the residual rate of the silica abrasive medium particles on the surface of the alumina wafer is lower than 3 particles/mu m 2 。
The polishing process and the polishing effect of the polishing composition of the invention are set forth below:
first, the polishing mechanism of silica sol to silica: in the chemical mechanical polishing process, the main function of the abrasive is to remove a softening layer generated on the surface of a workpiece to be polished by mechanical grinding, so as to expose an ultra-smooth surface. In the polishing process, the temperature of the polishing interface of the alumina wafer is increased, thereby promoting SiO 2 And the aluminum oxide and water react to form aluminosilicate. The aluminosilicate particles are larger and are removed from the surface of the wafer under the action of shearing force, in addition, the hardness of the aluminosilicate is slightly lower than that of SiO2, so that partial product is removed by SiO2 abrasive through mechanical action, and in short, the silica sol polishing alumina process at least comprises a superposition process of mechanical removal and chemical reaction, and the reaction formula which can be related in the process is as follows:
Al 2 O 3 + SiO 2 =Al 2 SiO 5
Al 2 O 3 + 2SiO 2 + 2H 2 O = Al 2 Si 2 O 7 •2H 2 O。
next, regarding the polishing liquid: the polishing solution disclosed by the invention is simpler in composition: silica sol grinding medium, complexing agent, surfactant, pH regulator and deionized water, wherein the mass percentages of the components are as follows: 10-25 wt% of silica sol grinding medium: the size of the silicon oxide abrasive medium particles is concentrated at 20-30nm, and D98 is less than or equal to 40nm;2.5-2.8wt.% complexing agent: p-hydroxyphenyl-beta-D-glucopyranoside; 0.5 to 0.7wt.% surfactant: hydroxyethyl ethylenediamine; pH regulator: diethylenetriamine, and adjusting the pH value to be in the range of 10-11; and the balance of deionized water.
The silica sol is an abrasive, is an important component of polishing solution, determines the mechanical action of polishing, influences the cleaning effect after polishing, greatly influences the polishing speed and the surface perfection of a polished surface, and has the main factors of polishing efficiency, namely abrasive grain size and abrasive concentration, and abrasive hardness and uniformity are determined by the type of the abrasive and the manufacturing process of the abrasive. As the most important component in the chemical mechanical polishing solution, the performance of the SiO2 abrasive plays a decisive role in the polishing result of the sapphire, but is extremely easy to agglomerate due to the high surface energy
The oversized abrasive is even precipitated, and oversized particles formed after agglomeration are extremely easy to scratch the surface of a workpiece, so that the oversized abrasive is a main cause of defects generated in the chemical mechanical polishing process of the workpiece. By trying silica sol with different particle sizes, the silicon polishing solution with the size concentrated at 20-30nm and D98 less than or equal to 40nm is finally found to have high removal rate and best polishing effect, and the obtained polished surface is smooth and has no scratches.
The main function of the surfactant is to reduce the surface energy of silica sol, prevent polishing scratch and low polishing efficiency caused by agglomeration, as mentioned above, the polishing solution nano silica sol of the invention is abrasive particles with the particle size of 20-30nm, but because the particle size is small, the surface area and the surface energy are large, the agglomeration is easy, and the performance of the polishing solution nano silica sol is directly affected, so that the improvement of the dispersibility and the stability of the polishing solution nano silica sol is the key for improving and stabilizing the polishing quality.
In the experimental process, in order to improve the material removal rate of CMP, the proportion of abrasive components in the polishing solution is continuously improved, meanwhile, the size of abrasive particles is continuously reduced to reduce the surface roughness after polishing, the surface area of abrasive particles is larger, the abrasive particles are easy to agglomerate into large particles in water or air, sometimes the particle size can reach more than 200nm, and the secondarily distributed particle size can even reach 500nm. These trends make abrasive particles poorly dispersible in polishing solutions, and thus hydroxyethyl ethylenediamine is added as a surfactant, which is indispensable in the preparation of polishing solutions, and which is added to the polishing solutions in advance after the introduction of silica sol in preference to other reagents.
pH regulator: in the alkaline silicon oxide CMP polishing solution, inorganic alkali is usually adopted, but metal ions exist in the inorganic alkali, so that the subsequent application of a wafer is easy to form great influence, such as the problem of increased leakage current of an integrated circuit device, and the like, therefore, organic alkali is usually used, can continuously release hydroxyl groups, supplement the hydroxyl groups consumed by chemical action in the polishing solution and maintain the stability of the pH value of the polishing solution. The two are not essentially different, but the invention takes the following treatment process into consideration, and preferably organic alkali diethylenetriamine is used as a pH regulator.
Complexing agent: the complexing agent has the main function of forming a complex with stable structure with metal ions in the chemical mechanical polishing process, so that the volume of the metal ions is increased, the removal is convenient, the forward progress of chemical reaction in the polishing process is promoted, and the polishing rate is improved.
The complexing agent adopted by the invention is p-hydroxyphenyl-beta-D-glucopyranoside (which is arbutin) with the following structural formula:
the p-hydroxyphenyl-beta-D-glucopyranoside is widely used in the field of cosmetics, and is rarely used as a complexing agent of polishing solution, such as CN107828341A, an antibacterial artificial stone polishing solution, which comprises the following raw materials in parts by weight: 5-10 parts of joint filling agent, 2-6 parts of antibacterial agent, 1-3 parts of antifouling agent, 5-8 parts of hyaluronic acid, 2-5 parts of arbutin, 4-8 parts of chitosan, 4-6 parts of magnesium sulfate, 2-5 parts of urea, 1-5 parts of pH regulator, 1-3 parts of surfactant and 50-100 parts of deionized water; the caulking agent adopts a mixture of potassium dihydrogen phosphate, fly ash and barium sulfate; the antibacterial agent comprises the following raw materials in parts by weight: 5-10 parts of zinc borate, 2-8 parts of viola philippica extract, 4-10 parts of balsam pear extract and 1-3 parts of chitin. The antibacterial artificial stone polishing solution can promote and maintain the brightness of the surface of the artificial stone, kill bacteria on the surface of the stone and inhibit bacterial growth for a long time, and has the antibacterial rate of 98.5% for escherichia coli and 99.3% for staphylococcus aureus; the preparation method is simple and is beneficial to market popularization. The arbutin has no specific effect disclosed in the invention, and according to the understanding of the applicant, the arbutin is a surface brightening agent or an antibacterial agent, and because the stone polishing process is mechanical polishing rather than chemical mechanical polishing, the effect of the arbutin in the invention has a very obvious limitation, namely, the arbutin is introduced into the chemical mechanical polishing liquid for the first time as a complexing agent.
As described above, the chemical mechanical polishing process is a process in which a chemical etching action and a mechanical grinding action are coupled with each other, the softening layer formed in the polishing process is Al (OH) 4-, and the p-hydroxyphenyl-beta-D-glucopyranoside is a pentahydroxy hybrid compound, and has extremely high complexing ability, and can be subjected to complexing reaction with metal ions such as iron, copper, zinc and the like to generate a soluble complex, so that the soluble complex is effectively complexed with the softening layer Al (OH) 4-, and the polishing removal rate of the substrate is effectively improved after the p-hydroxyphenyl-beta-D-glucopyranoside is subjected to complexing reaction with tetrahydroxy aluminate ions. Furthermore the presence of benzene rings and hybridization provides sufficient complexing space for complexation such that each hydroxyl group may become a ligand for the complexation reaction, forming a stable polycyclic complex product. In addition, the p-hydroxyphenyl-beta-D-glucopyranoside is easy to remove, and has positive effect on the subsequent removal of grinding media. .
Essence: the citrus essence, the lemon essence or the grape essence can be added with water-soluble essence for improving the cleaning effect and the smell of the polishing solution, improving the construction environment and being beneficial to physical and mental health.
The beneficial technical effects are as follows: (1) According to the polishing composition, the complexing capacity of the softening layer and the complexing agent is effectively improved by adding the p-hydroxyphenyl-beta-D-glucopyranoside complexing agent, the polishing removal efficiency is highest under an alkaline condition, and the obtained wafer has a smooth surface and low roughness.
(2) The polishing solution composition has the advantages of simple components, low residual rate of surface polishing medium and convenient post-polishing treatment.
Detailed Description
The preparation method of the polishing solution comprises the following steps:
(1) Dispersing silica sol grinding medium with particle size of 20-30nm in proper amount of deionized water, adding hydroxyethyl ethylenediamine surfactant while stirring, stirring at 100-150rpm for 10-15min at normal temperature to form stable suspension;
(2) Adding p-hydroxyphenyl-beta-D-glucopyranoside complexing agent into the suspension solution, stirring at the speed of 100-150rpm at the temperature of 30-35 ℃ for 2-3min, and supplementing the rest normal-temperature deionized water containing limonin;
(3) And adjusting the pH value of the solution to be within the range of 10-11 by using a diethylenetriamine pH regulator to obtain the wafer faint scent type polishing solution composition.
And (3) after polishing, placing the material into a 60W and 40KHz ultrasonic cleaner for 2-3min, wherein the solution in the ultrasonic cleaner is 50wt.% ethanol solution, and then drying.
The SMS-250 type table abrasive disc machine of the polishing equipment used in the invention has the experiment that the flow rate of the polishing liquid is 10 mL/min, the polishing rotating speed is 500 rpm, the polishing environment temperature is 25 ℃, and the polishing time is 15 min.
The material removal rate calculation formula: mrr= (M 0 -M 1 /ρSt)*107;
Wherein MRR is material removal rate (nm/min);
M 0 -the mass (g) of the wafer before polishing;
M 1 -the quality (g) of the sapphire wafer after polishing;
rho-sapphire wafer density (approximately3.97 g/cm) 2 ) ；
S-sapphire wafer surface area (≡20cm) 2 ) ；
t-polishing time (min).
The surface roughness was measured using a Dimension ICON atomic force microscope (Atomic Force Microscopy, AFM) manufactured by Bruker corporation, usa, and the surface topography of the sapphire wafer before and after polishing was characterized by selecting a region having a scanning area of 10 μm×10 μm.
Example 1
A polishing liquid composition:
10wt% silica sol;
2.5wt.% of a p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.5wt.% hydroxyethyl ethylenediamine surfactant;
0.01wt.% lemon essence;
diethylenetriamine pH adjustor to adjust ph=10;
and the balance of deionized water.
Example 2
A polishing liquid composition:
17.5wt% silica sol;
2.65wt.% of a p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.6wt.% hydroxyethyl ethylenediamine surfactant;
0.03wt.% lemon extract essence;
diethylenetriamine pH adjustor, adjusting ph=10.5;
and the balance of deionized water.
Example 3
A polishing liquid composition:
25wt% silica sol;
2.8wt.% of a p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.7wt.% hydroxyethyl ethylenediamine surfactant;
0.05wt.% lemon extract essence;
diethylenetriamine pH adjustor, adjusting ph=11;
and the balance of deionized water.
Example 4
A polishing liquid composition:
17.5wt% silica sol;
2.65wt.% of a p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.6wt.% hydroxyethyl ethylenediamine surfactant;
0.03wt.% lemon extract essence;
diethylenetriamine pH adjustor, adjusting ph=10.5;
and the balance of deionized water.
Example 5
A polishing liquid composition:
17.5wt% silica sol;
2.65wt.% of a p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.6wt.% hydroxyethyl ethylenediamine surfactant;
0.03wt.% lemon extract essence;
diethylenetriamine pH adjustor, adjusting ph=10.5;
and the balance of deionized water.
Comparative example 1. A polishing liquid composition:
17.5wt% silica sol;
0wt.% p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.6wt.% hydroxyethyl ethylenediamine surfactant;
0.03wt.% lemon extract essence;
diethylenetriamine pH adjustor, adjusting ph=10.5;
and the balance of deionized water.
Comparative example 2. A polishing liquid composition:
17.5wt% silica sol;
1wt.% of a p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.6wt.% hydroxyethyl ethylenediamine surfactant;
0.03wt.% lemon extract essence;
diethylenetriamine pH adjustor, adjusting ph=10.5;
and the balance of deionized water.
Comparative example 3. A polishing liquid composition:
17.5wt% silica sol;
3.2wt.% of a p-hydroxyphenyl- β -D-glucopyranoside complexing agent;
0.03wt.% lemon extract essence;
0.6wt.% hydroxyethyl ethylenediamine surfactant;
diethylenetriamine pH adjustor, adjusting ph=10.5;
and the balance of deionized water.
The surface roughness of the original wafer of the present invention was 6.237nm, and referring to examples 2-5, by adjusting the filling amount of the complexing agent, the polishing removal rate of the polishing liquid of the optimum formulation of the present invention was 1.94 μm/h, and the polishing roughness was 0.412nm, compared with comparative example 1, which was not added, and comparative examples 2-3, which were both too much and too little, which correspond to lower removal rates and polishing accuracy, and furthermore, it should be noted that if the complexing agent was added, there was still a large amount of silica adsorbed on the wafer surface after the post-polishing treatment, and removal was relatively difficult.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Those skilled in the art will appreciate that certain modifications and adaptations of the invention are possible and can be made under the teaching of the present specification. Such modifications and adaptations are intended to be within the scope of the present invention as defined in the appended claims.
Claims (2)
1. The preparation method of the faint scent type polishing solution composition is characterized by comprising the following steps of:
(1) Dispersing silica sol grinding medium with particle size of 20-30nm in proper amount of deionized water, adding hydroxyethyl ethylenediamine while stirring, stirring at 100-150rpm for 10-15min at normal temperature to form stable suspension;
(2) Adding p-hydroxyphenyl-beta-D-glucopyranoside into the suspension, stirring at the speed of 100-150rpm at the temperature of 30-35 ℃ for 2-3min, and supplementing the rest normal-temperature deionized water containing limonin;
(3) Adjusting the pH value of the solution to be within the range of 10-11 by using a diethylenetriamine pH regulator to obtain the wafer faint scent type polishing solution composition;
the fragrant polishing solution composition comprises the following components in percentage by mass:
10-25 wt% of silica sol grinding medium: the size of the silica abrasive medium particles is concentrated at 20-30nm, D 98 ≤40nm；
2.5-2.8wt.% p-hydroxyphenyl-beta-D-glucopyranoside;
0.5 to 0.7wt.% hydroxyethyl ethylenediamine;
0.01-0.05wt.% limonene essence;
pH regulator: diethylenetriamine, and adjusting the pH value to be in the range of 10-11;
and the balance of deionized water.
2. A fragrant polishing composition, characterized by being obtained by the method for preparing a fragrant polishing composition according to claim 1, wherein the polishing roughness ra=0.4-0.6 nm of an alumina wafer obtained by treating the fragrant polishing composition has a removal rate of 1.67-1.94 μm/h.
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