KR20160112136A - Polishing slurry composition - Google Patents
Polishing slurry composition Download PDFInfo
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- KR20160112136A KR20160112136A KR1020150037271A KR20150037271A KR20160112136A KR 20160112136 A KR20160112136 A KR 20160112136A KR 1020150037271 A KR1020150037271 A KR 1020150037271A KR 20150037271 A KR20150037271 A KR 20150037271A KR 20160112136 A KR20160112136 A KR 20160112136A
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- slurry composition
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
-
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
-
- 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
Description
The present invention relates to a polishing slurry composition.
As the design rule of the product is reduced, the aspect ratio (depth / floor width) is rapidly increasing due to the narrow width and height of the structure, and the influence of the scratches generated in the conventional 50- It affects the process more than 2 times. As a result, the influence of topography as well as scratches on the surface of the film was also enhanced. The most important factors to be considered in the polishing process are the amount of polishing and the quality of the polishing surface. Recently, as the semiconductor design rule is reduced, the importance of the quality of the polishing surface is maximized.
On the other hand, as the degree of integration of semiconductors has increased recently, a lower current leakage is required, and a high-permittivity dielectric and a metal gate structure have been devised to satisfy this demand. Aluminum has been widely used as a metal gate material in general. However, due to problems such as difficulty in complete deposition due to reduction in design rule and difficulty in polishing aluminum oxide having high hardness, much research has been conducted on using tungsten as a gate material have. However, it is indispensable to carry out a cleaning process for removing residual abrasive particles on the tungsten film surface after polishing by inducing adsorption between the abrasive particles and the tungsten film due to the surface potential difference during the polishing of the tungsten film. There is a problem that the dispersion stability is lowered and storage for a long time is difficult. Therefore, there is an increasing demand for development of polishing slurry compositions for tungsten film polishing.
An object of the present invention is to provide a polishing slurry composition having a high dispersion stability in an acidic region and capable of minimizing residual abrasive particles and metallic impurities on a tungsten film surface after polishing will be.
However, the problems to be solved by the present invention are not limited to the above-mentioned problems, and other matters not mentioned can be clearly understood by those skilled in the art from the following description.
According to the present invention, abrasive particles surface-modified with metal ions; Oxidant; And a pH adjusting agent.
The metal ion may be at least one selected from the group consisting of Al, Fe, Mn, Cu, Mg, Zn, Ni, Ca, And may include at least one selected from the group consisting of barium (Ba), vanadium (V), praseodymium (Pr), and ruthenium (Ru)
The abrasive particles may be negatively charged.
The abrasive particles may have a zeta potential of -20 mV to -100 mV.
Wherein the abrasive particles comprise at least one selected from the group consisting of a metal oxide coated with a metal oxide, an organic substance or an inorganic substance, and the metal oxide in a colloidal state, and the metal oxide is at least one selected from the group consisting of silica, ceria, zirconia, alumina, At least one selected from the group consisting of titania, barium titania, germania, manganese, and magnesia.
The abrasive grains may be 0.5 wt% to 10 wt% of the abrasive slurry composition.
The abrasive grains may have an average particle diameter of 80 nm to 500 nm.
The oxidizing agent is selected from the group consisting of hydrogen peroxide, hydrogen peroxide, urea hydrogen peroxide, urea, percarbonate, periodate, periodate, perchlorate, perchlorate, perbromate, perbromate, perborate, perborate, permanganate, permanganate, persulfate, At least one selected from the group consisting of bromine, chlorate, chlorite, chromate, iodate, iodate, ammonium peroxodisulfate, benzoyl peroxide, calcium peroxide, barium peroxide, sodium peroxide and peroxide Lt; / RTI >
The oxidizing agent may be 0.005 wt% to 5 wt% of the polishing slurry composition.
Wherein the pH adjusting agent is an inorganic acid or an inorganic acid salt containing at least one selected from the group consisting of nitric acid, hydrochloric acid, phosphoric acid, sulfuric acid, hydrofluoric acid, bromic acid, iodic acid and salts thereof; And organic acids such as formic acid, malonic acid, maleic acid, oxalic acid, acetic acid, citric acid, adipic acid, acetic acid, propionic acid, fumaric acid, lactic acid, salicylic acid, pimelic acid, benzoic acid, succinic acid, phthalic acid, butyric acid, glutaric acid, An organic acid or an organic acid salt containing at least one selected from the group consisting of glycolic acid, lactic acid, aspartic acid, tartaric acid and salts thereof.
The pH of the polishing slurry composition may be in the range of 1 to 5.
The polishing slurry composition had a polishing rate of 10 A / min. To 1,000 A / min. Of the tungsten film polishing rate.
The polished surface of the tungsten-containing film using the polishing slurry composition may have a peak to valley (PV) value of 100 nm or less and a surface roughness of 10 nm or less.
The polishing slurry composition according to the present invention has high stability in acidity as the surface of the abrasive grains is chemically bonded to the surface of the abrasive grains and the abrasive grains have the same charge as the surface of the tungsten film surface, Particles and metal impurities are not generated, and the abrasive particle adsorption on the tungsten surface after polishing can be improved.
FIG. 1 shows the results of polishing surface analysis of a tungsten film using the polishing slurry composition of an embodiment of the present invention.
FIG. 2 (A) is a photograph of a surface after polishing a tungsten film using the polishing slurry composition according to an embodiment of the present invention, and FIG. 2 (B) It is the surface photograph after polishing of membrane quality.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the following description of the present invention, detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear. In addition, terms used in this specification are terms used to appropriately express the preferred embodiments of the present invention, which may vary depending on the user, the intention of the operator, or the practice of the field to which the present invention belongs. Therefore, the definitions of these terms should be based on the contents throughout this specification. Like reference symbols in the drawings denote like elements.
Throughout the specification, when an element is referred to as "comprising ", it means that it can include other elements as well, without excluding other elements unless specifically stated otherwise.
Hereinafter, the polishing slurry composition of the present invention will be specifically described with reference to examples and drawings. However, the present invention is not limited to these embodiments and drawings.
According to the present invention, abrasive particles surface-modified with metal ions; Oxidant; And a pH adjusting agent.
The polishing slurry composition according to the present invention has a high stability in acidity as the surface of the abrasive grains is chemically bonded to the surface of the abrasive grains and the surface of the abrasive grains has the same charge as the surface of the tungsten film surface in the acidic state, Abrasive particle impurities are not generated and the abrasive particle adsorption on the tungsten film surface can be improved.
The metal ion may be at least one selected from the group consisting of Al, Fe, Mn, Cu, Mg, Zn, Ni, Ca, And may include at least one selected from the group consisting of barium (Ba), vanadium (V), praseodymium (Pr), and ruthenium (Ru)
When the abrasive grains are suspended in the polishing slurry composition through chemical bonding with the metal ions, the net electric charge becomes negatively charged abrasive grains.
The abrasive particles may have a negative electric charge and have a zeta potential of -20 mV to -100 mV. The zeta potential used in the present invention is a measured value of static charge at the surface of the abrasive grains. The magnitude of the zeta potential is an indication of the tendency of abrasive particles to repel other particles or surfaces with similar charges. The greater the magnitude of the zeta potential between the two materials, the stronger the repulsive force. For example, particles with large zeta potentials repel other negatively charged particles or surfaces. In the acidic region, the surface of the abrasive grains has the same negative charge as the surface of the tungsten film, thereby improving adsorption by repulsive force.
Wherein the abrasive particles comprise at least one selected from the group consisting of a metal oxide coated with a metal oxide, an organic substance or an inorganic substance, and the metal oxide in a colloidal state, and the metal oxide is at least one selected from the group consisting of silica, ceria, zirconia, alumina, Titania, barium titania, germania, manganese, and magnesia, but it may preferably be colloidal silica.
The abrasive grains may be 0.5 wt% to 10 wt% of the abrasive slurry composition. When the content of the abrasive grains in the polishing slurry composition is less than 0.5% by weight, there is a concern that the polishing target film, for example, tungsten can not be sufficiently polished at the time of polishing and the planarization rate may be lowered. If it is exceeded, it may cause defects such as defects and scratches.
The abrasive grains may have an average particle diameter of 80 nm to 500 nm. The abrasive grains may be blended with two types of abrasive grains having different sizes depending on calcination conditions and / or milling conditions, and may have a bimodal grain size distribution. The three types of abrasive grains may be mixed to form three kinds It may be that the abrasive grains having different peaks are mixed and have a broad size distribution. The relatively large abrasive grains and the relatively small abrasive grains can be mixed to have better dispersibility and the effect of reducing the scratch on the wafer surface can be expected.
The oxidizing agent is selected from the group consisting of hydrogen peroxide, hydrogen peroxide, urea hydrogen peroxide, urea, percarbonate, periodate, periodate, perchlorate, perchlorate, perbromate, perbromate, perborate, perborate, permanganate, permanganate, persulfate, At least one selected from the group consisting of bromine, chlorate, chlorite, chromate, iodate, iodate, ammonium peroxodisulfate, benzoyl peroxide, calcium peroxide, barium peroxide, sodium peroxide and peroxide Lt; / RTI > Among them, it is preferable to use hydrogen peroxide in view of the oxidative power, the dispersion stability of the polishing slurry composition, and economical efficiency.
The oxidizing agent may be 0.005 wt% to 5 wt%, preferably 0.05 wt% to 1 wt%, of the polishing slurry composition. When the oxidizing agent is less than 0.005 wt% in the polishing slurry composition, the polishing rate and the etching rate with respect to tungsten may be lowered. When the oxidizing agent is more than 5 wt%, the oxide film on the tungsten surface becomes hard, The oxide film grows and the topography can have a bad characteristic due to corrosion and erosion of tungsten.
The pH adjusting agent may further include a substance used to prevent corrosion of a metal or a polishing machine and to realize a pH range in which metal oxidation is easily caused. Examples of the pH adjusting agent include nitric acid, hydrochloric acid, phosphoric acid, sulfuric acid, An inorganic acid or an inorganic acid salt containing at least one selected from the group consisting of an acid, an iodic acid and a salt thereof; And organic acids such as formic acid, malonic acid, maleic acid, oxalic acid, acetic acid, citric acid, adipic acid, acetic acid, propionic acid, fumaric acid, lactic acid, salicylic acid, pimelic acid, benzoic acid, succinic acid, phthalic acid, butyric acid, glutaric acid, An organic acid or an organic acid salt containing at least one selected from the group consisting of glycolic acid, lactic acid, aspartic acid, tartaric acid and salts thereof.
The pH adjusting agent may be added in an amount to control the pH of the polishing slurry composition, and the pH of the polishing slurry composition according to the present invention may be in the range of pH from 1 to 5, preferably from 2 to 4 .
The polishing slurry composition of the present invention is acidic, and the abrasive particles surface-modified with the metal ion can have high stability in the polishing slurry composition.
The polishing slurry composition may be one for polishing a tungsten-containing substrate. The tungsten-containing substrate includes tungsten and tantalum, titanium, ruthenium, hafnium, and other refractory metals, nitrides and silicides thereof.
Using the polishing slurry composition of the present invention, a polishing rate of 10 A / min. To 1,000 ANGSTROM / min, preferably 100 ANGSTROM / min. And a tungsten film polishing rate of 700 A / min.
The polished surface of the tungsten-containing film using the polishing slurry composition may have a peak to valley (PV) value of 100 nm or less and a surface roughness of 10 nm or less. The peak-to-valley value and the degree of surface roughness can be measured with an atomic force microscope.
The polishing slurry composition of the present invention has a high stability in acidity and the abrasive particles have the same charge as the tungsten film surface and can improve the adsorption to metallic impurities. In addition, since it is effective to improve the topography of tungsten, it is possible to improve yields due to metal shorts and etch failures caused by film-like topography during tungsten polishing, and to enable a next-generation high integration process . In addition, since only the topography of tungsten is removed, it is possible to prevent the tungsten from being wasted by proceeding the superficial edge, and the surface such as erosion phenomenon, dishing phenomenon and formation of metal layer residue on the surface of the object to be polished The defect can be significantly reduced.
Hereinafter, the present invention will be described in detail with reference to the following examples and comparative examples. However, the technical idea of the present invention is not limited or limited thereto.
[Example]
Water-based colloidal silica abrasive grains having an average particle size of 80 to 100 nm were surface-modified with metal ions (Fe ions). The surface modified abrasive grains were mixed with 0.5 wt% hydrogen peroxide, and nitric acid was added to prepare a mixture of pH 2.5. The prepared mixture was stirred for 2 to 10 hours and filtered using a filter having a pore size of 0.5 mu m to prepare a polishing slurry composition.
[Comparative Example]
A polishing slurry composition was prepared under the same conditions as in Example except that alkoxide-based silica abrasive grains were used and that the abrasive grains were not surface-modified with metal ions.
The tungsten wafer was polished under the following polishing conditions using the polishing slurry compositions of Examples and Comparative Examples.
[Polishing condition]
1. Polishing equipment:
2. Polishing pad: IC 100 (Dow)
3. Head speed: 60 rpm
4. Platen Speed: 65 rpm
5. Pressure: 3 psi
6. Flow rate: 200 ml / min
7. Polishing target film: Tungsten (blanket wafer in which titanium nitride (TiN) and tungsten are sequentially deposited on a 200 mm polycrystalline silicon substrate in a thickness of 50 nm and 5,000 nm, respectively)
(1) Property evaluation
Table 1 below shows physical properties of the polishing slurry compositions of Comparative Examples and Examples of the present invention.
(nm)
(mV)
(㎲)
(Å / min)
Referring to Table 1, it was confirmed that the abrasive grains of the examples had a high negative electric charge with high zeta potential and were stable in acidity. As a result of polishing using the polishing slurry compositions of Examples and Comparative Examples, the polishing rate of the polishing slurry composition of the Example was 20% lower than that of the polishing slurry composition of the Comparative Example. This is due to the charge repulsion between the abrasive particles and the tungsten film surface.
(2) Evaluation of metal impurities
Table 2 shows results of inductively coupled plasma mass spectrometry (ICP MS) measurements of the polishing slurry compositions of the comparative examples and examples of the present invention.
Referring to Table 2, the abrasive slurry compositions of the example comprising colloidal silica based on water glass have relatively high Na and Al contents in the analysis of metallic impurities. In the case of Al, the element is chemically bonded to Si-O and Si in the form of Si-O-Al and Si-Al-Si, metal impurity factor).
(3) CMP After the process tungsten Papil Surface analysis ( XPS ) evaluation
FIG. 1 shows the results of polishing surface analysis of a tungsten film using the polishing slurry composition of an embodiment of the present invention. The tungsten film surface was confirmed by X-ray photoelectron spectroscopy (XPS). Table 3 below shows the XPS analysis results.
Referring to FIGS. 1 and 3, it can be seen that when polishing is carried out using the surface-modified abrasive particles of the embodiment, the binding energy is low at the tungsten film surface after polishing, and metal impurities (Al and Na) are not observed . It was confirmed that not only the improvement of dispersion stability and adsorption property but also the problem of metal impurities can be solved in the polishing of tungsten film.
(4) Evaluation of dispersion stability
Table 4 below shows the dispersion stability evaluation of the polishing slurry composition according to the comparative example and the example of the present invention for 3 months. The dispersion stability evaluation confirmed the increase of the size of the abrasive particles due to agglomeration of the abrasive particles for 3 months.
(nm)
(nm)
(nm)
Referring to Table 4, it was confirmed that the polishing slurry composition of the example maintained stability for 3 months, and in the case of the comparative example, it was confirmed that the size of the abrasive grains due to agglomeration of the particles increased from 1 month.
Table 5 below shows the evaluation of the dispersion stability for 7 days under extreme conditions of the polishing slurry compositions according to the comparative examples and examples of the present invention. The increase in the size of the abrasive grains due to agglomeration of the abrasive grains was confirmed at an extreme condition of 60 ° C for 7 days.
(nm)
(nm)
(nm)
(nm)
(nm)
(nm)
(nm)
Referring to Table 5, as in the 3-month stability evaluation, the polishing slurry composition of the Example shows no change in the abrasive particle size, and the abrasive slurry composition of the Comparative Example shows an increase in the abrasive grain size.
(5) Adsorption property evaluation
The adsorption properties of the polishing slurry compositions according to the comparative examples and the examples of the present invention were evaluated by performing deionized water cleaning (with ultrasonic waves) after dipping at room temperature for 10 minutes. FIG. 2 (A) is a photograph of a surface after polishing a tungsten film using the polishing slurry composition according to an embodiment of the present invention, and FIG. 2 (B) It is the surface photograph after polishing of membrane quality. 2 (A), using the polishing slurry composition according to the embodiment of the present invention, the surface after polishing of the tungsten film is polished by a repulsive force due to the same negative surface zeta potential of the abrasive grains and the tungsten film, It can be confirmed that no adsorption has occurred. Referring to FIG. 2 (B), in the case of the abrasive particles of the polishing slurry composition of Comparative Example in which the zeta potential value is a positive value, a large amount of adsorption occurs due to the surface potential difference with the tungsten film surface having a negative zeta potential value in acidity .
While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. This is possible. Therefore, the scope of the present invention should not be limited by the described embodiments, but should be determined by the equivalents of the appended claims, as well as the appended claims.
Claims (13)
Oxidant; And
pH adjusting agents;
≪ / RTI >
The metal ion may be at least one selected from the group consisting of Al, Fe, Mn, Cu, Mg, Zn, Ni, Ca, Wherein the polishing slurry composition contains at least any one selected from the group consisting of barium (Ba), vanadium (V), praseodymium (Pr), and ruthenium (Ru).
Wherein the abrasive grains are negatively charged.
Wherein the abrasive particles have a zeta potential of -20 mV to -100 mV.
The above-
At least one selected from the group consisting of a metal oxide coated with a metal oxide, an organic or inorganic material, and a metal oxide in a colloidal state,
Wherein the metal oxide comprises at least one selected from the group consisting of silica, ceria, zirconia, alumina, titania, barium titania, germania, manganese, and magnesia.
Abrasive slurry composition.
Wherein the abrasive grains are from 0.5 wt% to 10 wt% of the abrasive slurry composition.
Wherein the abrasive grains have an average particle diameter of 80 nm to 500 nm.
Preferably,
Hydrogen peroxide, hydrogen peroxide, urea hydrogen peroxide, urea, percarbonate, periodate, periodate, perchlorate, perchlorate, perbromate, perbromate, perborate, perborate, permanganate, permanganate, persulfate, bromate, Wherein the polishing composition comprises at least one selected from the group consisting of chlorites, chlorates, chromates, iodates, iodic acid, ammonium peroxodisulfate, benzoyl peroxide, calcium peroxide, barium peroxide, sodium peroxide and peroxide. Slurry composition.
Wherein the oxidizing agent is 0.005 wt% to 5 wt% of the polishing slurry composition.
The pH adjusting agent may be,
An inorganic acid or an inorganic acid salt containing at least one selected from the group consisting of nitric acid, hydrochloric acid, phosphoric acid, sulfuric acid, hydrofluoric acid, bromic acid, iodic acid and salts thereof; And
But are not limited to, formic, malonic, maleic, oxalic, acetic, adipic, citric, adipic, acetic, propionic, fumaric, lactic, salicylic, pimelic, benzoic, succinic, An organic acid or an organic acid salt containing at least any one selected from the group consisting of acid, lactic acid, aspartic acid, tartaric acid and salts thereof;
≪ / RTI > wherein the polishing slurry composition further comprises at least one selected from the group consisting of:
Wherein the polishing slurry composition has a pH in the range of from 1 to 5.
The polishing slurry composition had a polishing rate of 10 A / min. To 1,000 A / min. Of the tungsten film polishing rate.
Wherein the polished surface of the tungsten-containing film using the polishing slurry composition has a peak to valley (PV) value of 100 nm or less and a surface roughness of 10 nm or less.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190137656A (en) * | 2018-06-01 | 2019-12-11 | 주식회사 케이씨텍 | Polishing slurry composition |
| KR20210050246A (en) * | 2019-10-28 | 2021-05-07 | 주식회사 케이씨텍 | High removal rate oxide film polishing slurry composition |
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2015
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190137656A (en) * | 2018-06-01 | 2019-12-11 | 주식회사 케이씨텍 | Polishing slurry composition |
| KR20210050246A (en) * | 2019-10-28 | 2021-05-07 | 주식회사 케이씨텍 | High removal rate oxide film polishing slurry composition |
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