CN106929858A - Chemical mechanical polishing of metals slurry - Google Patents
Chemical mechanical polishing of metals slurry Download PDFInfo
- Publication number
- CN106929858A CN106929858A CN201511029138.5A CN201511029138A CN106929858A CN 106929858 A CN106929858 A CN 106929858A CN 201511029138 A CN201511029138 A CN 201511029138A CN 106929858 A CN106929858 A CN 106929858A
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- CN
- China
- Prior art keywords
- acid
- mechanical polishing
- chemical mechanical
- metals
- phosphate
- 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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- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims 1
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims 1
- BVWCKYAYMBDPIP-UHFFFAOYSA-N NC=1C=C(C=C(C1)N)C=CC1=CC=CC=C1 Chemical class NC=1C=C(C=C(C1)N)C=CC1=CC=CC=C1 BVWCKYAYMBDPIP-UHFFFAOYSA-N 0.000 claims 1
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- 235000009508 confectionery Nutrition 0.000 claims 1
- 150000002460 imidazoles Chemical class 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 claims 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 98
- 239000010949 copper Substances 0.000 abstract description 93
- 229910052802 copper Inorganic materials 0.000 abstract description 91
- 230000007547 defect Effects 0.000 abstract description 6
- 239000000356 contaminant Substances 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 description 23
- 235000012431 wafers Nutrition 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 230000004888 barrier function Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229940024606 amino acid Drugs 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000021523 carboxylation Effects 0.000 description 3
- 238000006473 carboxylation reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007517 polishing process Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 229920006231 aramid fiber Polymers 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 150000003851 azoles Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 150000003852 triazoles Chemical class 0.000 description 2
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 1
- XYJLPCAKKYOLGU-UHFFFAOYSA-N 2-phosphonoethylphosphonic acid Chemical compound OP(O)(=O)CCP(O)(O)=O XYJLPCAKKYOLGU-UHFFFAOYSA-N 0.000 description 1
- MZWDAEVXPZRJTQ-WUXMJOGZSA-N 4-[(e)-(4-fluorophenyl)methylideneamino]-3-methyl-1h-1,2,4-triazole-5-thione Chemical compound CC1=NNC(=S)N1\N=C\C1=CC=C(F)C=C1 MZWDAEVXPZRJTQ-WUXMJOGZSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- DCXYFEDJOCDNAF-UHFFFAOYSA-N Asparagine Natural products OC(=O)C(N)CC(N)=O DCXYFEDJOCDNAF-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- 241001272567 Hominoidea Species 0.000 description 1
- DCXYFEDJOCDNAF-REOHCLBHSA-N L-asparagine Chemical compound OC(=O)[C@@H](N)CC(N)=O DCXYFEDJOCDNAF-REOHCLBHSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 235000009582 asparagine Nutrition 0.000 description 1
- 229960001230 asparagine Drugs 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000005605 benzo group Chemical group 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229960001484 edetic acid Drugs 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- MCXBMLBTPQEQJP-UHFFFAOYSA-N potassium;sodium;dinitrate Chemical compound [Na+].[K+].[O-][N+]([O-])=O.[O-][N+]([O-])=O MCXBMLBTPQEQJP-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- RDRCCJPEJDWSRJ-UHFFFAOYSA-N pyridine;1h-pyrrole Chemical compound C=1C=CNC=1.C1=CC=NC=C1 RDRCCJPEJDWSRJ-UHFFFAOYSA-N 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The present invention provides a kind of chemical mechanical polishing slurry and its application for copper, and the slurry includes：(a) abrasive grains (b) complexing agent (c) oxidant (d) corrosion inhibitor (e) phosphate ester surfactant.Using the removal rate that can keep copper higher of slurry of the invention, improve after polishing the butterfly depression of copper cash and cross the defects such as throwing window, the copper surface contaminant after polishing is few, corrosion-free.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing slurry and its application, more particularly to a kind of change for copper
Learn mechanical polishing material and its application.
Background technology
With the development of semiconductor technology, the microminiaturization of electronic unit contains number in one integrated circuit
Transistor in the millions.Running incorporates the transistor that can be switched rapidly of such vast number,
The reduction of signal transmission speed, and electric current can be caused to transmit using traditional aluminium or aluminium alloy interconnection line
Need to consume mass energy in journey, the development of semiconductor technology is also counteracts that on this definite meaning.In order to enter
One step develops, and people begin look for having the use of the material substitution aluminium of electrical properties higher.It is well known that
The resistance of copper is small, with good electric conductivity, this increases the transmission speed of signal between transistor in circuit,
Smaller parasitic capacitance ability is may also provide, reduces sensitiveness of the circuit for electromigration.These electricity are excellent
Point all causes that copper shows good development prospect in semiconductor technology development.
But it was found that copper can be migrated or diffusion way enters into collection in the ic manufacturing process of copper
Into the transistor area of circuit, so as to the performance to semiconductor transistor has a negative impact, thus copper
Interconnection line can only be manufactured with mosaic technology, i.e.,：Groove is formed in ground floor, copper resistance is filled in groove
Barrier and copper, form plain conductor and cover on the dielectric layer.Then by chemically-mechanicapolish polishing dielectric
Unnecessary copper/copper barrier layer is removed on layer, and single interconnection line is left in groove.The chemically mechanical polishing of copper
Process is generally divided into 3 steps, and the 1st step is first with lower pressure higher, with fast and efficient removal speed
Rate removes substantial amounts of copper on substrate surface, and the 2nd step is pressure under being reduced when soon close to barrier layer, drop
Low removal rate polishes remaining metallic copper and is parked in barrier layer, and the 3rd step is removed with barrier polishing solution again
Barrier layer and part of dielectric layer and metallic copper, realize planarization.
On the one hand copper polishing will as early as possible remove copper unnecessary on barrier layer, and polishing is on the other hand reduced as far as possible
The butterfly of copper cash is recessed afterwards.Before copper polishing, metal level has portion concave above copper cash.During polishing,
Copper on dielectric material is easy to be removed under prevailing pressure higher, and the polishing pressure suffered by the copper of recess
Power is lower than prevailing pressure, and copper removal rate is small.With the carrying out of polishing, the difference in height of copper can be gradually reduced,
Reach planarization.But in polishing process, if the chemical action of copper polishing fluid is too strong, static corrosion
Speed is too high, even if then the passivating film of copper is at low pressures, and (such as copper cash recess) is also easy to be removed,
Causing planarization efficiency reduces, the butterfly depression increase after polishing.
With the development of integrated circuit, on the one hand, in traditional IC industries, in order to improve integrated level,
Reducing energy consumption, shortens time delay, and line width is more and more narrow, and the number of plies of wiring is also more and more, in order to protect
Demonstrate,prove the performance and stability of integrated circuit, requirement to copper CMP also more and more higher.It is required that
Polish pressure is reduced in the case of the removal rate for ensureing copper, the planarization of copper line surface, control table is improved
Planar defect.On the other hand, due to physical limitation, line width can not infinitely reduce, and semicon industry is no longer
Merely rely on one chip integrated more devices to improve performance, and turn on multi-chip package.
Silicon hole (TSV) technology makes as one kind by between chip and chip, between wafer and wafer
Vertical conducting, realizes the state-of-the-art technology that interconnects between chip and obtains being widely recognized as industrial quarters.TSV energy
The density for enough making chip stack in three-dimensional is maximum, and appearance and size is minimum, substantially improve chip speed and
The performance of low-power consumption.Current TSV techniques are to combine traditional IC techniques to form the copper for running through silicon base
Perforation, i.e., fill copper and realize conducting in TSV openings, and unnecessary copper is also required to using chemistry after filling
Mechanical polishing removal reaches planarization.It is different from traditional IC industry, because silicon hole is very deep, after filling
The copper of excess surface generally has a few to tens of micron of thickness.In order to quickly remove these unnecessary copper.Generally need
There is copper removal rate very high, while the surface smoothness after polishing is good.In order that copper is in semiconductor
Preferably applied in technology, people continuously attempt to the improvement of new polishing fluid.
Chinese patent CN1256765C provides a kind of containing citric acid, potassium citrate and chelating organic acid
The polishing fluid of buffer system.CN1195896C is used and is contained oxidant, carboxylate such as ammonium citrate, mill
The polishing fluid of slurry liquid, a kind of optional triazole or triazole derivative.CN1459480A provides one kind
The chemical mechanical polishing liquid of copper, it comprises film forming agent and coalescents：Film forming agent is mixed by highly basic and acetic acid
The cushioning liquid being combined into is constituted, and coalescents are potassium nitrate (sodium) salt.United States Patent (USP) US552742
There is provided a kind of chemical mechanical polishing of metals slurry, including it is a kind of containing aramid fiber silica, alkane polysiloxanes,
The surfactant of polyoxyalkylene ether and its copolymer.US6821897B2 provides a kind of using containing poly-
The copper chemical mechanical polishing method of the polishing agent of compound complexing agent, it uses the polymer containing negative electrical charge, its
Include thiosulfonic acid and its salt, sulfate, phosphoric acid, phosphate, phosphate etc..And US5527423
Chemical mechanical polishing of metals slurry, including a kind of surfactant：It is aramid fiber siloxanes, polysiloxanes, poly-
One or more in oxyalkylene ether and its copolymer.
Technology in above-mentioned patent, in the polishing process of copper, all make every effort to reduce the local spot corrosion of layers of copper and
Corrosion, controls static etch rate, so as to preferably remove layers of copper, improves the polishing speed of copper, and obtain
Obtain copper-connection flatness well.Above-mentioned patent overcomes above-mentioned copper in polishing process to a certain extent
Problem encountered, but effect is not obvious, has defect on copper surface after use, and flatness is low, and
And there is saucerization greatly and crosses the problem for throwing window narrows in copper cash after polishing；Polishing speed is not high enough, it is impossible to
It is applied to the technique higher to removal rate requirement.
The content of the invention
The invention provides a kind of chemical mechanical polishing of metals slurry, added with phosphorus in the polishing slurries
Acid esters is the surfactant of main component, can keep the polishing speed of copper higher, after reducing copper polishing
Saucerization, improve the planarization on surface, Strengthening and Polishing effect, the copper surface contaminant after polishing is few,
The defect such as corrosion-free.
Chemical mechanical polishing of metals slurry of the present invention is achieved through the following technical solutions its purpose：
A kind of chemical mechanical polishing of metals slurry, including abrasive grains, complexing agent, corrosion inhibitor, oxygen
Agent and phosphate ester surfactant, wherein, the phosphate ester surfactant is mono phosphoric acid ester esters
One or more in the composition of compound and phosphate diester class compound.Wherein, the phosphate monoester
The mass percent of class compound and phosphate diester class compound is 70：30-30：70.The mono phosphoric acid ester
As indicated with 1, the structural formula of phosphate diester compound is as indicated with 2 for the structural formula of ester type compound：
Wherein X=RO, RO- (CH2CH2O)n,RCOO-(CH2CH2O)n；R is glyceryl or C8~C22
Alkyl, alkylbenzene etc.；N=2~30, M=H, K, NH4, Na or (CH2CH2O)1~3NH3~1。
Wherein, when R is C8~C22Alkyl when, the phosphate ester surfactant be polyoxyethylene
Ether phosphate or its salt, preferably alkylpolyoxyethylene phosphate, alkylpolyoxyethylene
Phosphate kalium salt, Steareth phosphate, Steareth phosphate kalium salt.
When R be alkylbenzene when, surfactant be APES phosphate or its salt, it is preferably pungent
Base phenol polyethenoxy ether phosphate, thermally coupled distillation columns, octadecyl phenol polyethenoxy ether
Phosphoric acid ester sodium.
Above-mentioned chemical mechanical polishing of metals slurry, wherein, the content of the phosphate ester surfactant
It is mass percent 0.0005-1%, preferably mass percent 0.001-0.5%.
Chemical mechanical polishing of metals slurry of the invention, wherein, the abrasive grains are silica, oxygen
Change silica, ceria, titanium dioxide and the macromolecule abrasive grains of aluminium, adulterated al or aluminium coating
In one or more.
Above-mentioned chemical mechanical polishing of metals slurry, wherein, the particle diameter of the abrasive grains is 20~200nm,
The reference area of the abrasive grains is 5-1000m2/g。
Chemical mechanical polishing of metals slurry of the invention, wherein, the content of the abrasive grains is quality hundred
Divide and compare 0.1-20%.
Chemical mechanical polishing of metals slurry of the invention, wherein, the complexing agent be amino acid and its salt,
One kind in ammonia carboxylation compound and its salt, organic carboxyl acid and its salt, organic phospho acid and its salt and organic amine or
It is several.Wherein, the amino acid is glycine, alanine, valine, leucine, proline, benzene
Alanine, tyrosine, tryptophan, lysine, arginine, histidine, serine, aspartic acid,
Threonine, glutamic acid, asparagine, glutamine；The ammonia carboxylation compound and its salt be nitrilotriacetic acid,
Ethylenediamine tetra-acetic acid, 1,2-diaminocyclohexane tetraacetic acid, EDDS, diethylene triamine pentacetic acid (DTPA) and three
One or more in the hexaacetic acid of ethene four；The organic carboxyl acid is acetic acid, oxalic acid, citric acid, wine
One kind in stone acid, malonic acid, succinic acid, malic acid, lactic acid, gallic acid and sulfosalicylic acid or
It is several；Described organic phosphoric acid is 2- phosphonobutane -1,2,4- tricarboxylic acids, ATMP, hydroxyl
Base ethylene-diphosphonic acid, ethylene diamine tetra methylene phosphonic acid, diethylene triamine pentamethylene phosphonic, 2- hydroxyethylidene diphosphonic acid bases
One or more in acetic acid, ethylene diamine tetra methylene phosphonic acid and many ether methylenephosphonic acids of polyamino；It is described to have
Machine amine be ethylenediamine, diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, triethylene tetramine,
One or more in TEPA.Wherein, amino-acid salt, ammonia carboxylation adduct salt, organic carboxylate,
Organic phosphonate is sylvite, sodium salt or ammonium salt.
Above-mentioned chemical mechanical polishing of metals slurry, wherein, the content of the complexing agent is mass percent
0.05-10%.Preferably mass percent 0.1-5%
Chemical mechanical polishing of metals slurry of the invention, wherein, described oxidant is hydrogen peroxide, mistake
Oxidation urea, peroxyformic acid, Peracetic acid, persulfate, percarbonate, periodic acid, perchloric acid, height
One or more in boric acid, potassium permanganate and ferric nitrate.Wherein, the content of the oxidant is quality
Percentage 0.05-10%.
Chemical mechanical polishing of metals slurry of the invention, wherein, described corrosion inhibitor is nitrogen azoles, miaow
One or more in azoles, thiazole, pyridine and pyrimidines.Wherein, nitrogen azole compounds are benzene
And triazole, 5- methyl benzotriazazoles, 5- carboxy benzotriazoles, 1- hydroxyls-BTA, 1,
2,4- triazoles, 3- amino -1,2,4- triazoles, 4- amino -1,2,4- triazoles, 3,5- diaminos
Base -1,2,4- triazoles, 5- carboxyl -3- amino -1,2,4- triazoles, 3- amino -5- sulfydryl -1,2,
4- triazoles, 5- acetic acid -1H- tetrazoles, 5- methyl tetrazoles, 5- phenyl tetrazole, 5- amino -1H- four
One or more in nitrogen azoles and 1- phenyl -5- sulfydryls-tetrazole；The glyoxaline compound is benzo miaow
One or more in azoles, 2-mercaptobenzimidazole.Described thiazole compound is 2- sulfydryls-benzo thiophene
Azoles, 2- dimercaptothiodiazoles and 5- amino-2-mercapto phenyl formic -1, one or more in 3,4- thiadiazoles；The pyrrole
Pyridine is one or more in 2,3- diamino-pyridines, PA and 2- pyridine carboxylic acids；It is described phonetic
Pyridine is 2- aminopyrimidines.
Above-mentioned chemical mechanical polishing of metals slurry, wherein, the content of the corrosion inhibitor is quality hundred
Divide than 0.001-2%, preferably mass percent 0.005-1%.
The pH value of chemical mechanical polishing of metals slurry of the invention is 3-11, preferably 4-8.
Also include pH adjusting agent, viscosity modifier, froth breaking in above-mentioned chemical mechanical polishing of metals slurry
The conventional additive in this areas such as agent, bactericide.
When preparing above-mentioned chemical mechanical polishing of metals slurry, the other components in addition to oxidant can be prepared
Into concentrating sample, it is diluted to concentration range of the invention with deionized water and adds oxidant using preceding.
Chemical mechanical polishing of metals slurry of the invention is in the chemically mechanical polishing of the base material containing copper
Using.Be the advantage is that using chemical mechanical polishing of metals slurry of the present invention：
1. by adding phosphate ester surfactant so that polishing slurries of the invention are at low pressures
The reduction of copper removal rate, and still there is copper removal rate higher at elevated pressures, improve production capacity.
2. chemical mechanical polishing of metals slurry of the invention enhances the polishing effect of copper, after reducing polishing
The butterfly depression of copper cash, improved throwing window.
Brief description of the drawings
Figure 1A and 1B are the copper wafer surface SEM after being polished using polishing slurries of the invention
Photo
Fig. 2A and 2B are to be polished using polishing slurries of the invention and the copper wafer surface scanning electron after soaking
Microphotograph
Specific embodiment
The present invention is expanded on further below by specific embodiment.
Embodiment 1~49
Table 1 gives the embodiment 1~49 of chemical mechanical polishing liquid of the invention, is formulated by given in table,
Other components in addition to oxidant are well mixed, mass percent to 100% is supplied with water.Use KOH
Or HNO3Adjust required pH value.Using preceding oxidizer, it is well mixed.
The embodiment 1~49 of table 1
Effect example
Table 2 gives embodiment 50~71 and the comparative example 1~9 of chemical mechanical polishing liquid of the invention,
It is formulated by given in table, the other components in addition to oxidant is well mixed, quality percentage is supplied with water
Than to 100%.With KOH or HNO3Adjust required pH value.Using preceding oxidizer, mix
Close uniform.
The comparative example 1~9 of table 2 and embodiment 50~71
Using contrast polishing fluid 1~8 and polishing fluid of the invention 50~65, to empty piece copper (Cu) chip and
The copper chip for having figure is polished.The removal rate of the copper of gained is shown in Table 3, the burnishing stick of graphical wafer
Butterfly-type depression value and the copper residual of part and copper billet are shown in Table 4.
Empty piece copper wafer polishing condition：1~3psi of lower pressure；Polishing disk and rubbing head rotating speed 93/87rpm,
Polishing pad IC1010, polishes flow velocity 150ml/min, and polishing machine platform is 8 " Mirra.
Figuratum copper wafer polishing procedure condition：Polishing disk and rubbing head rotating speed 93/87rpm, polishing pad
IC1010, polishes flow velocity 150ml/min, and polishing machine platform is 8 " Mirra.Phase is used on polishing disk 1
Then the figuratum copper chip of lower press polish answered is used on polishing disk 2 again to remaining copper about 3000A
The copper of residual is removed and crosses throwing 20 seconds by lower pressure accordingly.Measured with XE-300P AFMs
The butterfly-type depression value of the copper billet of 80um*80um on figuratum copper chip, it is figuratum after observation polishing
The residual condition of copper is shown in Table 4 on copper chip
Copper removal rate under the different polish pressures of the polishing fluid of table 3
Copper residual after butterfly depression value and polishing under the figuratum copper chip difference polishing condition of table 4 at 80um*80um copper billets
Can be learnt from form 3 and 4：Compared with polishing fluid 1~2 is contrasted, mono phosphoric acid ester esters chemical combination is added
The removal rate of the contrast polishing fluid 3 of thing is substantially reduced, it is impossible to effectively remove copper removal, adds phosphoric acid double
The removal rate of the contrast polishing fluid 4 of ester compounds is basically unchanged, so the butterfly of copper after polishing cannot be reduced
Shape is recessed.It is 80 that contrast polishing fluid 5 adds single di esters compound ratio：20 phosphoric acid ester
After compound, removal rate and the butterfly depression of copper are reduced, but figure wafer has copper to remain after polishing, will
Influence the electrical property and yield of wafer.It is 20 that contrast polishing fluid 6 adds single di esters compound ratio：
After 80 phosphate compounds, although the removal rate of copper higher can be kept, but to butterfly depression
Reduction is not very effective.And single di esters is added in chemical mechanical polishing of metals slurry 50~65 of the invention
Compound quality percentage is 70：30~30：Can effectively be dropped after 70 phosphate ester surfactant
Removal rate of the low copper under low pressure, and it is little on the removal rate influence under lower pressure higher.
This characteristic can cause that polishing fluid remains to obtain more smooth throwing in the case where removal rate higher is kept
Optical surface, substantially increases production efficiency, and the butterfly depression value of the copper billet after polishing is reduced again, and
Figure crystal column surface is without copper residual (being shown in Table 4) after polishing.
Figure wafer after being polished with embodiment 57 soaks 30 minutes in polishing fluid, uses scanning electron
Copper line surface situation before the immersion of micro- sem observation after (after polishing) and immersion, see accompanying drawing 1A, 1B,
2A, 2B, it can be seen that the wafer surface after being polished with the polishing fluid is corrosion-free, zero defect.
Soaked 30 minutes in polishing fluid, copper cash still without substantially corrosion and defect, illustrates polishing fluid of the invention
There is the ability of very strong suppression metal erosion.
It is empty to empty piece copper (Cu) chip using contrast polishing fluid 9 and polishing fluid of the invention 66~71
Piece silica wafers, empty piece tantalum chip and the copper chip for having figure are polished.The polishing speed of gained
And the butterfly-type depression value of copper billet is shown in Table 5.
Empty piece polishing condition：1~3psi of lower pressure；Polishing disk and rubbing head rotating speed 93/87rpm, polishing pad
IC1010, polishes flow velocity 150ml/min, and polishing machine platform is 8 " Mirra.
Figuratum copper wafer polishing procedure condition：Polishing disk and rubbing head rotating speed 93/87rpm, polishing pad
IC1010, polishes flow velocity 150ml/min, and polishing machine platform is 8 " Mirra.3psi is used on polishing disk 1
The figuratum copper chip of lower press polish to remaining copper about 5000A, then used on polishing disk 2 again
The copper removal that the lower pressure of 2psi will be remained.Figuratum copper is measured with XE-300P AFMs
Butterfly-type depression value on chip at the copper cash of 10um/10um (copper cash/silica).
Butterfly depression value after the empty piece removal rate of the polishing fluid of table 5 and the polishing condition of figuratum copper chip and polishing
Can be learnt from form 5：Compared with polishing fluid 9 is contrasted, chemical mechanical polishing of metals slurry of the invention
Material 66~68 can remain to obtain more smooth polished surface in the case where removal rate higher is kept, by
Embodiment 69~71 is visible, and the polishing fluid is adjustable in copper removal rate it is also possible to provide higher
Silica and tantalum removal rate.The polishing fluid can meet different application demands.
It should be appreciated that wt% of the present invention refers to weight/mass percentage composition.
Specific embodiment of the invention has been described in detail above, but it is intended only as example, this hair
It is bright to be not restricted to particular embodiments described above.To those skilled in the art, it is any to this
The equivalent modifications that carry out of invention and substitute also all among scope of the invention.Therefore, this hair is not being departed from
The impartial conversion and modification made under bright spirit and scope, all should be contained within the scope of the invention.
Claims (22)
1. a kind of chemical mechanical polishing of metals slurry, including abrasive grains, complexing agent, corrosion inhibitor, oxygen
Agent and phosphate ester surfactant, it is characterised in that the phosphate ester surfactant is
One or more in the composition of mono phosphoric acid ester ester type compound and phosphate diester class compound, wherein,
The mass percent of mono phosphoric acid ester ester type compound and phosphate diester class compound is 30：70-70：30.
2. chemical mechanical polishing of metals slurry as claimed in claim 1, it is characterised in that the mono phosphoric acid ester
The structural formula of ester type compound such as formula 1, the structural formula such as formula 2 of the phosphate diester class compound
Wherein：X=RO, RO- (CH2CH2O)n,RCOO-(CH2CH2O)n；R be glyceryl or
The alkyl or alkylbenzene of C8~C22, n=2~30, M=H, K, NH4,Na,(CH2CH2O)1~3NH3~1。
3. chemical mechanical polishing of metals slurry as claimed in claim 2, the mono phosphoric acid ester ester type compound and
Phosphate diester class compound is one or more in polyoxyethylene ether phosphate and its salt, alkyl phenol
One or more in polyoxyethylene ether phosphate and its salt.
4. chemical mechanical polishing of metals slurry as claimed in claim 3, the polyoxyethylene ether phosphate and
Its salt be alkylpolyoxyethylene phosphate, alkylpolyoxyethylene phosphate kalium salt,
Steareth phosphate, Steareth phosphate kalium salt；The alkane
Base phenol polyethenoxy ether phosphate and its salt are OPEO phosphate, polyoxyethylene nonyl phenyl
Ethene ether phosphate, octadecyl phenol polyethenoxy ether phosphoric acid ester sodium.
5. chemical mechanical polishing of metals slurry as claimed in claim 1, it is characterised in that the phosphate
The content of class surfactant is mass percent 0.0005-1%.
6. chemical mechanical polishing of metals slurry as claimed in claim 5, it is characterised in that the phosphate
The content of class surfactant is mass percent 0.001-0.5%.
7. chemical mechanical polishing of metals slurry as claimed in claim 1, it is characterised in that the grinding
Grain is silica, ceria, the dioxy of silica, aluminum oxide, adulterated al or aluminium coating
Change titanium, one or more in macromolecule abrasive grains.
8. chemical mechanical polishing of metals slurry as claimed in claim 1, it is characterised in that the grinding
The particle diameter of grain is 20-200nm.
9. chemical mechanical polishing of metals slurry as claimed in claim 1, it is characterised in that the grinding
The content of grain is mass percent 0.1-20%.
10. chemical mechanical polishing of metals slurry as claimed in claim 1, it is characterised in that the complexing agent
For amino acid and its salt, aminoxatyl complex and its salt, organic carboxyl acid and its salt, organic phosphoric acid and its
One or more in salt and organic amine.
11. metallochemistry polishing slurries as claimed in claim 10, it is characterised in that the amino-acid salt,
Aminoxatyl complex salt, organic carboxylate and organic phosphate are sylvite, sodium salt or ammonium salt.
12. metallochemistry polishing slurries as claimed in claim 10, it is characterised in that the amino acid is sweet
Propylhomoserin, alanine, valine, leucine, proline, phenylalanine, tyrosine, tryptophan,
Lysine, arginine, histidine, serine, aspartic acid, threonine, glutamic acid, asparagus fern
One or more in acid amides, glutamine；Aminoxatyl complex is nitrilotriacetic acid, ethylenediamine tetrem
Acid, 1,2-diaminocyclohexane tetraacetic acid, EDDS, diethylene triamine pentacetic acid (DTPA) and triethylene four
One or more in hexaacetic acid；The organic carboxyl acid is acetic acid, oxalic acid, citric acid, winestone
One kind in acid, malonic acid, succinic acid, malic acid, lactic acid, gallic acid and sulfosalicylic acid
Or it is several；The organic phosphoric acid be 2- phosphonobutane -1,2,4- tricarboxylic acids, ATMP,
1-hydroxy ethylidene-1,1-diphosphonic acid, ethylene diamine tetra methylene phosphonic acid, diethylene triamine pentamethylene phosphonic, 2- hydroxyls
One kind or several in phosphono-acetic acid, ethylene diamine tetra methylene phosphonic acid and many ether methylenephosphonic acids of polyamino
Kind；The organic amine is many ethylenediamine, diethylenetriamine, pentamethyl-diethylenetriamine, many ethene
One or more in amine, triethylene tetramine, TEPA.
13. chemical mechanical polishing of metals slurries as claimed in claim 1, it is characterised in that the complexing agent
Content be mass percent 0.05-10%.
14. chemical mechanical polishing of metals slurries as claimed in claim 13, it is characterised in that the complexing agent
Content be mass percent 0.1-5%.
15. chemical mechanical polishing of metals slurries as claimed in claim 1, it is characterised in that the oxidant
For hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic acid, persulfate, percarbonate,
One or more in periodic acid, perchloric acid, boric acid high, potassium permanganate and ferric nitrate.
16. chemical mechanical polishing of metals slurries as claimed in claim 1, it is characterised in that the oxidant
Content be mass percent 0.05-10%.
17. chemical mechanical polishing of metals slurries as claimed in claim 1, it is characterised in that the corrosion suppression
Preparation is one or more in nitrogen azoles, imidazoles, thiazole, pyridine and pyrimidines.
18. chemical mechanical polishing of metals slurries as claimed in claim 17, it is characterised in that the nitrogen azole
Compound be BTA, 5- methyl benzotriazazoles, 5- carboxy benzotriazoles, 1- hydroxyls-
BTA, 1,2,4- triazoles, 3- amino -1,2,4- triazoles, 4- amino -1,2,
4- triazoles, 3,5- diaminostilbenes, 2,4- triazoles, 5- carboxyl -3- amino -1,2,4- triazoles,
3- amino -5- sulfydryl -1,2,4- triazoles, 5- acetic acid -1H- tetrazoles, 5- methyl tetrazoles, 5-
One or more in phenyl tetrazole, 5- amino -1H- tetrazoles and 1- phenyl -5- sulfydryls-tetrazole.
The glyoxaline compound is one or more in benzimidazole and 2-mercaptobenzimidazole；It is described
Thiazole compound be 2- Mercapto-benzothiazoles, 2- dimercaptothiodiazoles and 5- amino-2-mercapto phenyl formic -1,3,
One or more in 4- thiadiazoles；The pyridine be 2,3- diamino-pyridines, PA and
One or more in 2- pyridine carboxylic acids；The pyrimidine is 2- aminopyrimidines.
19. chemical mechanical polishing of metals slurries as claimed in claim 1, it is characterised in that the corrosion suppression
The content of preparation is mass percent 0.001-2%.
20. chemical mechanical polishing of metals slurries as claimed in claim 19, it is characterised in that the corrosion suppression
The content of preparation is mass percent 0.005-1%.
21. chemical mechanical polishing of metals slurries as claimed in claim 1, it is characterised in that the grinding
Grain specific surface area is 5-1000m2/g。
A kind of base of the 22. chemical mechanical polishing of metals slurries as any one of claim 1-21 in cupric
Chemically mechanical polishing application on material.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511029138.5A CN106929858A (en) | 2015-12-31 | 2015-12-31 | Chemical mechanical polishing of metals slurry |
| PCT/CN2016/111684 WO2017114301A1 (en) | 2015-12-31 | 2016-12-23 | Chemical and mechanical polishing slurry for metal |
| TW105143241A TW201723112A (en) | 2015-12-31 | 2016-12-26 | Metal chemical mechanical polishing slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511029138.5A CN106929858A (en) | 2015-12-31 | 2015-12-31 | Chemical mechanical polishing of metals slurry |
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| CN106929858A true CN106929858A (en) | 2017-07-07 |
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ID=59225632
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511029138.5A Pending CN106929858A (en) | 2015-12-31 | 2015-12-31 | Chemical mechanical polishing of metals slurry |
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| Country | Link |
|---|---|
| CN (1) | CN106929858A (en) |
| TW (1) | TW201723112A (en) |
| WO (1) | WO2017114301A1 (en) |
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| CN107629449A (en) * | 2017-08-24 | 2018-01-26 | 金寨宏伟新材料有限公司 | A kind of method that PA6 one-levels feed back prepares master batch |
| CN108250234A (en) * | 2016-12-28 | 2018-07-06 | 安集微电子（上海）有限公司 | A kind of synthesis technology of phosphate ester surfactants and its application |
| CN109401631A (en) * | 2017-08-17 | 2019-03-01 | 弗萨姆材料美国有限责任公司 | Chemical mechanical planarization (CMP) compositions and methods for copper and through silicon via (TSV) applications |
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| CN103865400A (en) * | 2012-12-10 | 2014-06-18 | 安集微电子（上海）有限公司 | Application of organic phosphate surfactant in self-stopping polishing |
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| CN103160207A (en) * | 2011-12-16 | 2013-06-19 | 安集微电子（上海）有限公司 | Metal chemico-mechanical polishing sizing agent and application thereof |
| CN103866326A (en) * | 2012-12-10 | 2014-06-18 | 安集微电子（上海）有限公司 | Chemo-mechanical polishing slurry for metal, and its application |
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2017114301A1 (en) | 2017-07-06 |
| TW201723112A (en) | 2017-07-01 |
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