CN106433479B - The control method of multi-layer copper metallization cobalt barrier layer surface roughness - Google Patents
The control method of multi-layer copper metallization cobalt barrier layer surface roughness Download PDFInfo
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- CN106433479B CN106433479B CN201610576241.XA CN201610576241A CN106433479B CN 106433479 B CN106433479 B CN 106433479B CN 201610576241 A CN201610576241 A CN 201610576241A CN 106433479 B CN106433479 B CN 106433479B
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- polishing
- surface roughness
- barrier layer
- polishing fluid
- copper metallization
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
Abstract
The invention belongs to CMP arts, more particularly to a kind of control method of multi-layer copper metallization cobalt barrier layer surface roughness, alkalescence polishing liquid is configured first, then in flow 100-500ml/min, 15-30 DEG C of temperature, ramming head revolving speed are 57-150rpm, revolving speed of dumping is 63-150rpm, carry out polishing 1-5min under the process conditions that polish pressure is 6.89-27.56kpa；The alkalescence polishing liquid includes: the 0.1%-1% that amount of chelant accounts for polishing fluid gross mass；The dosage of nonionic surface active agent is the 1-5% of polishing fluid gross mass；The Si02Dosage accounts for the 1% of polishing fluid gross mass, and the final pH value of the polishing fluid is 8-12；The problem of mostly using acid polishing slurry the method overcome control cobalt barrier layer surface roughness existing during existing copper metallization chemical mechanical polishing and include oxidant.
Description
Technical field
The invention belongs to CMP art more particularly to a kind of multi-layer copper metallization cobalt barrier layer surface roughness
Control method.
Background technique
Nearly ten years, the integrated characteristic size experience of Giga large scale integration (GLSI) great scale
From 0.18 μm to the development course of 20nm, this indicates integrated circuit, and oneself is entered the nanoscale epoch.Currently, the U.S.
Inter company integrated circuit fabrication process has reached 14nm technology node, integrated level reach DRAM64G or 90,000,000 transistor/
cm2.Semi-conductor industry proposes it to chemical-mechanical planarization (CMP) technique of crystal column surface with the rapid development of Moore's Law
More stringent requirement, mainly since the further miniaturization of device fabrication size is to multi-layer copper metallization surface finish requirements
Further increase and continually introduced with novel stop layer material.After 14nm and following technology node, copper-connection
The number of plies also requires the blocking effect not only having had up to 13 layers or more, to the barrier layer of protection thin copper film, more requires have smaller thickness
Degree.The features such as cobalt is because of its high chemical stability, high rigidity, which becomes novel stop layer material, has good development prospect
Surface roughness is an important parameter in great scale integrated circuit manufacture in GLSI multilayer wiring CMP,
For characterizing the quality of CMP front and rear surfaces quality, the surface roughness after polishing is excessively high, will cause noise increase, electrical characteristics one
Cause property is poor, will affect device frequency characteristic such as increases the RC retardation ratio time, to influence integrated level, reliability, quality product rate and drop
Inexpensive surface roughness is lower to illustrate that the surface quality after polishing is higher, also illustrates the polishing fluid used and process conditions are most
It is preferred that selecting.So controlling the technical problem that surface roughness is always CMP in great scale integrated circuit manufacturing.
Patent CN102516875B and CN102304327A is each provided with a kind of polishing of polishing process based on metal Co
Liquid, the polishing fluid are acid (pH value range 3-5), separately include oxidant, abrasive grains, chelating agent, thiazole suppression
The water of preparation and surplus.But experiment discovery, in the acid polishing slurry containing oxidant, barrier material cobalt is easy to molten
Solution, causes the desorption of ditch buried copper, and make the surface roughness of cobalt very big.So developing a kind of control of cobalt surface roughness
Method is very necessary.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, during the existing copper metallization chemical mechanical polishing of solution
The problem of existing control cobalt barrier layer surface roughness mostly uses acid polishing slurry and includes oxidant, and a kind of multilayer is provided
The control method of thin copper film cobalt barrier layer surface roughness.
The present invention to achieve the above object, using following technical scheme:
A kind of control method of multi-layer copper metallization cobalt barrier layer surface roughness, includes the following steps:
1) it is formulated for reducing the polishing fluid of GLSI multi-layer copper metallization cobalt barrier layer surface roughness:
A. chelating agent deionized water is diluted 10-100 times；
B. nonionic surfactant is inclined into the solution of step a) formation, this is constantly stirred in the process；
C. the SiO for being 20-50nm by partial size2It is configured to the abrasive material hydrosol that mass fraction is 0.1-20%；
D. the obtained solution of step b) being poured into the solution that step c) is obtained, this is constantly stirred in the process, to
Deionized water is added after being thoroughly mixed and carries out constant volume；
2) in flow 100-500ml/min, 15-30 DEG C of temperature, ramming head revolving speed are 57-150rpm, revolving speed of dumping is 63-
150rpm, polish pressure be 6.89-27.56kpa process conditions under carry out polishing 1-5min；
Wherein, the amount of chelant accounts for the 0.1%-1% of polishing fluid gross mass；The use of nonionic surface active agent
Amount is the 1-5% of polishing fluid gross mass；The SiO2Dosage be polishing fluid gross mass 0.05%-10%；The throwing
The final pH value of light liquid is 8-12；
The nonionic surface active agent is OII-7((C10H21-C6H4-O-CH2CH2O)7-H)、OII-10((C10H21-
C6H4-O-CH2CH2O)10- H), 0-20, JFC, fatty alcohol polyoxyethylene ether, one kind of polyoxyethylene alkyl amine, alkylol phthalein amine
Or several mixing.
The chelating agent is triethanolamine, diethylamine, tetrahydroxyethyl-ethylene diamine, beta-hydroxyethyl ethylenediamine, ethylenediamine tetraacetic
One or several kinds of mixing of acetic acid-four-tetrahydroxyethyl-ethylene diamine.
Preferably, chelating agent deionized water extension rate is 20 times, and chelating agent is tetrahydroxyethyl-ethylene diamine, and chelating agent is used
Amount accounts for the 0.5% of polishing fluid gross mass, nonionic surfactant OII-10((C10H21-C6H4-O-CH2CH2O)10- H), it is non-
Ionic surfactant dosage is the 2% of polishing fluid gross mass, the SiO2Average grain diameter is 20-50nm, and abrasive material is water-soluble
The mass fraction of glue is 2%, SiO2Dosage accounts for the 1% of polishing fluid gross mass, and the final ph of the polishing fluid is 9-10；
Polishing technological conditions in the step 2) are as follows:
Operating pressure: 6.89kpa；Rubbing head/polishing disk rotating speed: 57/63rpm；Flow: 300mL/min, polishing time are
1min, 25 DEG C of temperature.
Compared with prior art, the beneficial effects of the present invention are:
The nonionic surface active agent has stronger penetrating power, it can penetrate into wafer surface and adsorbate
Between, and constantly extend, and adsorbate is held up, be conducive to polishing fluid and transport away reactant and product；It is non-ionic
Surfactant molecule, quickly in piece sublist face drawout, forms the protective layer of one layer of even compact, favorably using wetting action
It is cleaned after polishing；Nonionic surface active agent can be accelerated to polish the mass transfer of product in polishing fluid, so that chip
Removal rate at barrier layer surface convex-concave is different, is conducive to reduce difference of height at bumps, reduces surface roughness, realize throwing
Optical surface planarization.
Meanwhile the abrasive material is the aqueous silica sol of partial size 20-50nm.Nanoscale SiO2Colloidal sol is ground as polishing fluid
Material, partial size is small, concentration is high, hardness is small, small to copper and load injury tolerance, and it is smooth, low can to reach high-speed, height for good dispersion degree
Damage polish, pollution is small, solves abrasive hardness great Yi scuffing, easily many drawbacks such as precipitating.
The chelating agent is triethanolamine, diethylamine, tetrahydroxyethyl-ethylene diamine, beta-hydroxyethyl ethylenediamine, ethylenediamine tetraacetic
The one or several kinds of acetic acid-four-tetrahydroxyethyl-ethylene diamine.Chelating agent can play buffer as polishing fluid pH adjusting agent
Effect, while being also used as complexing agent and synthesizing water-soluble macromolecular product with metal ion network, make reaction product small
Mechanism under can be detached from finished surface.
In short, the present invention has selected polishing fluid configuration process appropriate, which will not generate gel in configuration process
The phenomenon that, facilitate the configuration of solution and the progress of subsequent polishing process.The polishing fluid does not contain oxidant, overcomes polishing fluid
Stability problem, meanwhile, polishing fluid is alkalinity, overcomes that barrier material cobalt is easy to dissolve, cause the desorption of ditch buried copper,
And the problem for making the surface roughness of cobalt very big.
Detailed description of the invention
Fig. 1 is that nonionic surface active agent accelerates polishing product quality transmitting schematic diagram；
Fig. 2 is influence schematic diagram of the nonionic surface active agent to surface roughness；
Fig. 3 is influence schematic diagram of the various concentration nonionic surface active agent to cobalt barrier layer surface roughness.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, with reference to the accompanying drawing and most
The present invention is described in further detail for good embodiment.
Working principle: as shown in Figure 1, for reduced surface roughness, the present invention introduces nonionic in polishing fluid
Type surfactant (active matter i.e. in figure), this is because nonionic surface active agent has stronger penetrating power,
It can penetrate between polished surface and adsorbate, and constantly extend, be conducive to the reaction product product that polishing fluid carries polishing
It transports away.Nonionic surface active agent can accelerate the mass transfer of the reactant of convex, and recess is due to viscous flow thickness,
Reduce mass transfer.Just because of the presence of nonionic agent, so that cobalt stops the removal speed at synusia surface relief
Rate is different, as shown in Fig. 2, it is fast in 1,2,3 removal rate of convex, it is slow in 4,5,6,7 removal rate of recess.Be conducive to reduce recessed
Convex difference of height reduces surface roughness.
In addition, the hydrophilic radical of nonionic surface active agent almost accounts for the 2/3-4/5 of entire molecule, add into polishing fluid
Enter nonionic surface active agent, using wetting action quickly in piece sublist face drawout, forms the guarantor of one layer of even compact
Sheath, meanwhile, when nonionic surface active agent Molecular Adsorption, connect with nonpolar hydrocarbon chain with solid based on, and hydrophily
Group then extend in water, form prevent polishing product absorption physical barrier, be conducive to polishing after clean.
Embodiment 1: 1g chelating agent diethylamine is put into 100g deionized water and is diluted, is then poured into the solution
The nonionic surface active agent O of 10gII-7((C10H21-C6H4-O-CH2CH2O)7- H), it is stirred continuously, then will in the process
It is 20%SiO that these mixed solutions, which pour into the mass fraction that the average grain diameter of 500g is 20-50nm,2In the hydrosol, in the process not
Disconnected stirring until pour into completely.Deionized water is added after it is thoroughly mixed makes its solution quality reach 1000g, the polishing at this time
The pH value of liquid is 8-9, in operating pressure: 30.47kpa；Rubbing head/polishing disk rotating speed: 150/150rpm；Flow: 300mL/
Min, temperature use the rough surface on atomic force microscope barrier layer to polish 1min under 25 DEG C of technique after polishing
Degree, as a result a1 shows that roughness RMS is 9.8nm such as in Fig. 3.
Embodiment 2
5g chelating agent triethanolamine is put into 100g deionized water, the non-ionic of 20g is then poured into the solution
Surfactant OII-10((C10H21-C6H4-O-CH2CH2O)10- H), it is stirred continuously in the process, it is then that these mixing are molten
Liquid pours into the SiO that the 20-50nm mass fraction of 500g is 2%2In the hydrosol, it is stirred continuously in the process until pour into completely, to
A small amount of deionized water is added in it after being thoroughly mixed make its solution quality reach 1000g.The pH value of the polishing fluid is 9-10 at this time.So
Afterwards in operating pressure: 6.89kpa；Rubbing head/polishing disk rotating speed: 57/63rpm；Flow: 500mL/min, technique under will throw
Light 2min uses the surface roughness on atomic force microscope barrier layer after polishing, a2 shows that roughness RMS is in Fig. 3
3.57nm。
Embodiment 3
5g chelating agent-tetrahydroxyethyl-ethylene diamine is put into 100g deionized water, the non-of 20g is then poured into the solution
Ionic surfactant 0-20, is stirred continuously in the process, then these mixed solutions are poured into the 20-50nm mass of 500g
The SiO that score is 2%2In the hydrosol, it is stirred continuously in the process until pouring into completely.Deionized water is added after it is thoroughly mixed
Its solution quality is set to reach 1000g, the pH value of the polishing fluid is 9-10 at this time.Then in operating pressure: 6.89kpa；Rubbing head/
Polishing disk rotating speed: 57/63rpm；Flow: pattern piece is polished into 1min under the technique of 300ml/min, atomic force is used after polishing
The surface roughness on microexamination barrier layer, a3 shows that roughness RMS is 0.41nm in Fig. 3.
Embodiment 4
5g chelating agent-beta-hydroxyethyl ethylenediamine is put into 50g ionized water, then poured into the solution 50g it is non-from
Subtype surfactant alkylol phthalein amine, is stirred continuously in the process, then these mixed solutions is poured into the 20-50nm of 500g
The SiO that mass fraction is 3%2In the hydrosol, it is stirred continuously in the process until pouring into completely.After it is thoroughly mixed be added go from
Sub- water makes its solution quality reach 1000g.The pH value of the polishing fluid is 9-10 at this time.Then in operating pressure: 27.56kpa；It throws
Shaven head/polishing disk rotating speed: 100/100rpm；Flow: 100ml/min, technique under pattern piece polished into 3min, after polishing
With the surface roughness on atomic force microscope barrier layer, a4 shows that roughness RMS is 1.88nm in Fig. 3.
Embodiment 5
5g chelating agent-ethylenediamine tetra-acetic acid-four-tetrahydroxyethyl-ethylene diamine is put into 100g deionized water, then at this
The nonionic surface active agent fatty alcohol polyoxyethylene ether that 30g is poured into solution, is stirred continuously in the process, then by these
Mixed solution pours into the SiO that the 20-50nm mass fraction of 500g is 2%2In the hydrosol, it is stirred continuously in the process until falling completely
Enter.Deionized water is added after it is thoroughly mixed makes its solution quality reach 1000g.The pH value of the polishing fluid is 9-10 at this time.
Then in operating pressure: 6.89kpa；Rubbing head/polishing disk rotating speed: 57/63rpm；Flow: 300ml/min, technique under will
Pattern piece polishes 1min, the surface roughness on atomic force microscope barrier layer is used after polishing, a5 shows roughness in Fig. 3
RMS is 3.52nm.
Embodiment 6
10g chelating agent hydroxyethyl ethylenediamine is put into 100g deionized water, then poured into the solution 50g it is non-from
Subtype surfactant polyoxyethylene alkylamine, is stirred continuously in the process, then these mixed solutions are poured into the 20- of 500g
The SiO that 50nm mass fraction is 0.1%2In the hydrosol, it is stirred continuously in the process up to pouring into completely, is added after it is thoroughly mixed
Entering deionized water makes its solution quality reach 1000g.The pH value of the polishing fluid is 11-12 at this time.Then in operating pressure:
6.89kpa；Rubbing head/polishing disk rotating speed: 57/63rpm；Flow: 300ml/min, technique under pattern piece polished into 5min,
The surface roughness on atomic force microscope barrier layer is used after polishing, a6 shows that roughness RMS is 3.79nm in Fig. 3；
The surface roughness from Fig. 3, it can be seen that various concentration nonionic surface active agent is to cobalt barrier layer table
The influence of surface roughness, the addition of nonionic surface active agent have the surface roughness on polishing front and back cobalt barrier layer obviously
Improvement.Meanwhile from a3, it is apparent that nonionic surface active agent O-20 concentration is 20mL/L in the polishing fluid
When, surface of polished flatness is good, does not scratch substantially, and cobalt barrier layer surface roughness reaches minimum.This is primarily due to non-
Ionic surfactant can accelerate the mass transfer of reaction product and reactant, simultaneously because activating agent can make burnishing surface table
Face tension is remarkably decreased, and is reached wetting surface and is improved homogeneity, is made the reduction of surface scratch defect, can be proved to apply nonionic
Type surfactant, improves surface roughness really, and can achieve effectively control and improve improves barrier layer surface roughness
Effect.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (1)
1. a kind of control method of multi-layer copper metallization cobalt barrier layer surface roughness, which is characterized in that include the following steps: 5g
Chelating agent-tetrahydroxyethyl-ethylene diamine is put into 100g deionized water, and the non-ionic surface that 20g is then poured into the solution is living
Property agent O-20, be stirred continuously in the process, be then 2% by the 20-50nm mass fraction that these mixed solutions pour into 500g
SiO2In the hydrosol, it is stirred continuously in the process until pouring into completely；Deionized water is added after it is thoroughly mixed makes its solution matter
Amount reaches 1000g, and the pH value of the polishing fluid is 9-10 at this time；Then in operating pressure: 6.89kpa；Rubbing head/polishing disk turns
Speed: 57/63rpm；Flow: 1min is polished under the technique of 300ml/min, uses atomic force microscope barrier layer after polishing
Surface roughness.
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|---|---|---|---|---|
| CN1861320A (en) * | 2006-06-09 | 2006-11-15 | 河北工业大学 | Method for controlling disc-like pit during chemically mechanical polishing for ULSI multiple-layered copper wiring |
| CN1861321A (en) * | 2006-06-09 | 2006-11-15 | 河北工业大学 | Method for controlling planeness during chemically mechanical polishing for ULSI multiple-layered copper wiring |
| CN1864925A (en) * | 2006-06-09 | 2006-11-22 | 河北工业大学 | Method for controlling roughness in ULSI multi-layer copper metallization chemico-mechanical polishing |
| JP2012169510A (en) * | 2011-02-16 | 2012-09-06 | Nitta Haas Inc | Abrasive composition |
| CN104449398A (en) * | 2014-11-25 | 2015-03-25 | 河北工业大学 | Alkaline chemical mechanical polishing solution applicable to cobalt barrier layer |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861320A (en) * | 2006-06-09 | 2006-11-15 | 河北工业大学 | Method for controlling disc-like pit during chemically mechanical polishing for ULSI multiple-layered copper wiring |
| CN1861321A (en) * | 2006-06-09 | 2006-11-15 | 河北工业大学 | Method for controlling planeness during chemically mechanical polishing for ULSI multiple-layered copper wiring |
| CN1864925A (en) * | 2006-06-09 | 2006-11-22 | 河北工业大学 | Method for controlling roughness in ULSI multi-layer copper metallization chemico-mechanical polishing |
| JP2012169510A (en) * | 2011-02-16 | 2012-09-06 | Nitta Haas Inc | Abrasive composition |
| CN104449398A (en) * | 2014-11-25 | 2015-03-25 | 河北工业大学 | Alkaline chemical mechanical polishing solution applicable to cobalt barrier layer |
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