CN120572457A - Endpoint detection window and preparation method and application thereof - Google Patents
Endpoint detection window and preparation method and application thereofInfo
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- CN120572457A CN120572457A CN202511087415.1A CN202511087415A CN120572457A CN 120572457 A CN120572457 A CN 120572457A CN 202511087415 A CN202511087415 A CN 202511087415A CN 120572457 A CN120572457 A CN 120572457A
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- detection window
- endpoint detection
- polishing
- prepolymer
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Abstract
本发明属于抛光垫制备技术领域，具体涉及一种终点检测窗口及其制备方法和应用。所述终点检测窗口的硬度自外周至中心方向逐渐变大，所述终点检测窗口中心点具有最大邵氏硬度D1，所述终点检测窗口外周边缘点具有最小邵氏硬度D2，所述D1和D2满足：0＜D1‑D2≤2，自边缘向中心硬度逐渐升高，既能保证终点检测窗口与抛光层接触的边缘硬度差值无明显变化，又能防止因终点检测窗口偏软造成抛光过程发生变形，减少终点检测窗口与抛光层硬度差异而造成的划伤，从而改善抛光一致性。
The present invention belongs to the technical field of polishing pad preparation, and specifically relates to an endpoint detection window, a preparation method, and an application thereof. The hardness of the endpoint detection window gradually increases from the periphery to the center, with the center point of the endpoint detection window having a maximum Shore hardness D1 and the peripheral edge points of the endpoint detection window having a minimum Shore hardness D2, wherein D1 and D2 satisfy the following: 0 < D1-D2 ≤ 2. The hardness gradually increases from the edge to the center, thereby ensuring that the difference in hardness between the edge of the endpoint detection window and the polishing layer does not change significantly, preventing deformation during the polishing process due to a soft endpoint detection window, reducing scratches caused by the hardness difference between the endpoint detection window and the polishing layer, and thus improving polishing consistency.
Description
Technical Field
The invention belongs to the technical field of polishing pad preparation, and particularly relates to an end point detection window and a preparation method and application thereof.
Background
In integrated circuit fabrication, it is often desirable to eliminate and planarize the fine relief of the wafer surface, and chemical mechanical planarization or Chemical Mechanical Polishing (CMP) is a common technique used to planarize or polish workpieces.
During polishing, an endpoint detection system is often used to detect the polishing endpoint to determine when a desired planarization level is achieved. The in situ detection method uses a polishing pad with an end-point detection window as an entrance to the laser light during polishing to allow inspection of the wafer surface. In-situ optical endpoint indication techniques can be categorized as monitoring a single wavelength reflected light signal or multiple wavelengths reflected light signals, where the reflectance of the substrate changes as the composition at the substrate surface changes from one material to another, and this change in reflectance is used to monitor the CMP polishing endpoint. For chemical mechanical polishing pads, how to further improve the polishing uniformity during application is still one of the technical difficulties to be broken through in the art.
Disclosure of Invention
In order to solve the problem of inconsistent polishing of the existing chemical mechanical polishing pad, the invention provides an endpoint detection window, and a preparation method and application thereof.
For this purpose, the invention provides the following technical scheme.
The first aspect of the invention provides an end point detection window, the Shore hardness of the end point detection window gradually increases from the periphery to the center, the center point of the end point detection window has the maximum Shore hardness D1, the peripheral edge point of the end point detection window has the minimum Shore hardness D2, and the D1 and the D2 meet that the Shore hardness is 0< D1-D2 is less than or equal to 2. Illustratively, D1-D2 is 0.2, 0.5, 0.8, 1.2, 1.5, 1.8, etc.
As an alternative embodiment, D1 is 70-75D. Illustratively, D1 is 70D, 71D, 72D, 73D, 74D, 75D, etc.
The second aspect of the invention provides a preparation method of the end point detection window, which comprises the steps of mixing a first prepolymer and a first curing agent to obtain a first mixture, wherein the chain extension coefficient f 1 of the first mixture is 0.9< f 1 and less than or equal to 0.99, mixing a second prepolymer and a second curing agent to obtain a second mixture, the chain extension coefficient f 2 of the second mixture is 0.8< f 2 and less than or equal to 0.9, and casting and curing.
In the endpoint detection window provided by the invention, the first prepolymer and the second prepolymer can be self-made or commercially available, for example, at least one of Adiprene prepolymer L325, LF750D, LF751D, LF600D, LF700D, LF950A, LFG963A, LF1950A and the like.
As an alternative embodiment, the first prepolymer has a mass content of unreacted NCO of 8-11%;
As an alternative embodiment, the second prepolymer has a mass content of unreacted NCO of 8-11%.
As an alternative embodiment, the first prepolymer has a mass content of unreacted NCO of 8.5 to 10.5%;
As an alternative embodiment, the second prepolymer has a mass content of unreacted NCO of 8.5 to 10.5%;
As an alternative embodiment, the first prepolymer is identical to the second prepolymer. I.e., the first prepolymer and the second prepolymer are prepared from the same raw material.
As an alternative embodiment, the starting material of the first prepolymer comprises isocyanate, and the isocyanate comprises at least one of dicyclohexylmethane diisocyanate, 4-diphenylmethane diisocyanate, isophorone diisocyanate and toluene diisocyanate;
As an alternative embodiment, the raw material of the second prepolymer comprises isocyanate, and the isocyanate comprises at least one of dicyclohexylmethane diisocyanate, 4-diphenylmethane diisocyanate, isophorone diisocyanate and toluene diisocyanate;
In the present invention, the raw material of the first prepolymer and/or the second prepolymer further includes polyether polyol, and the molecular weight of the polyether polyol may be, but is not limited to, 650-2000, such as 650, 1000, 1500, 2000, etc.
As an alternative embodiment, the first curing agent includes a hydroxyl-based curing agent and/or an amino-based curing agent;
As an alternative embodiment, the first curing agent includes at least one of ethylene glycol, propylene glycol, butylene glycol, 2-methyl-1, 3-propanediol, pentylene glycol, 3-methyl-1, 5-pentylene glycol, hexylene glycol, 4 '-methylenebis (2-chloroaniline), 4' -methylenebis (3-chloro-2, 6-diethylaniline), diethyltoluenediamine, 5-tert-butyl-2, 4-toluenediamine, 3-tert-butyl-2, 6-toluenediamine, 5-tert-amyl-2, 4-toluenediamine;
As an alternative embodiment, the second curing agent includes a hydroxyl-based curing agent and/or an amino-based curing agent;
As an alternative embodiment, the second curing agent includes at least one of ethylene glycol, propylene glycol, butylene glycol, 2-methyl-1, 3-propanediol, pentylene glycol, 3-methyl-1, 5-pentylene glycol, hexylene glycol, 4 '-methylenebis (2-chloroaniline), 4' -methylenebis (3-chloro-2, 6-diethylaniline), diethyltoluenediamine, 5-tert-butyl-2, 4-toluenediamine, 3-tert-butyl-2, 6-toluenediamine, 5-tert-amyl-2, 4-toluenediamine.
In a third aspect, the present invention provides a polishing pad comprising the endpoint detection window described above or the endpoint detection window made by the preparation method described above.
In the present invention, the end point detection window can be a monolithic window or a plug-in window in the polishing pad.
As an alternative embodiment, a stacked polishing layer and buffer layer are included, the endpoint detection window extending through the polishing layer and the buffer layer.
As an alternative embodiment, the polishing layer surface is provided with a plurality of grooves.
In the polishing pad provided by the invention, the polishing layer comprises a segmented block copolymer. The segmented block copolymer includes copolymers of hard segments and/or soft segments, for example, one or more of polyethylene oxide, poly (ether ester) block copolymers, polyamides, polyvinyl alcohol, polyvinylpyrrolidone, polyvinylpyridine, polyacrylic acid, polymethacrylic acid, polyaspartic acid, styrene polymers, epoxy-based polymers, maleic anhydride methyl vinyl ether copolymers, and the like.
The material of the buffer layer is a material known in the art. Optionally, the material of the buffer layer includes one or more of textile material, nonwoven material, polyurethane foam material, etc., such as felt material, spunbond material, needled material, etc., and also includes one or more of polymer impregnated felt material (e.g., polyurethane impregnated felt material), textile material (e.g., thick flannel material).
Optionally, the polishing pad further comprises an adhesive layer positioned between the polishing layer and the buffer layer. The adhesive layer is at least one of pressure-sensitive adhesive, reactive hot melt adhesive and the like, wherein the reactive hot melt adhesive is at least one of polyolefin, ethylene vinyl acetate, polyamide, polyester, polyurethane, polyvinyl chloride or epoxy resin and the like, and the pressure-sensitive adhesive is at least one of propenyl adhesive (PSAV) or rubber-based adhesive (PSA 8) and the like.
Alternatively, the grooves function to conduct the polishing liquid, polishing debris, and the like. The number of grooves is not particularly limited in the present invention. For example, the polishing layer surface can be provided with a plurality of grooves, which can be selected from concentric grooves (e.g., circular, spiral, etc.), curvilinear grooves, cross-hatched grooves (e.g., arranged in an X-Y grid on the polishing layer surface, e.g., in a checkered groove pattern), regular shapes (e.g., hexagonal, triangular, etc.), tread patterns, irregular designs or combinations, and the like.
When the polishing pad is used, the element to be polished is pressed on the polishing pad for chemical mechanical polishing, and the element to be polished can be a pattern sheet, a plating film sheet, a copper sheet and the like. During polishing, the element to be polished and the polishing pad are polished with relative motion provided. The specific operation of chemically mechanical polishing the element to be polished, the polishing apparatus, the polishing process, etc. can be referred to the prior art.
In a fourth aspect, the present invention provides a polishing pad for polishing a semiconductor substrate, a magnetic substrate, or an optical substrate.
The technical scheme of the invention has the following advantages:
1. According to the end point detection window provided by the invention, the hardness of the end point detection window gradually increases from the periphery to the center, the center point of the end point detection window has the maximum Shore hardness D1, the peripheral edge point of the end point detection window has the minimum Shore hardness D2, the D1 and the D2 meet that 0< D1-D2 are less than or equal to 2, the hardness gradually increases from the edge to the center, the difference value of the edge hardness of the end point detection window, which is contacted with the polishing layer, is not obviously changed, deformation in the polishing process caused by the soft bias of the end point detection window can be prevented, and scratch caused by the difference of the hardness of the end point detection window and the polishing layer is reduced, so that the polishing consistency is improved. The polishing layer in the polishing pad comprises microsphere components besides the raw materials such as prepolymer and curing agent, and the end point detection window is high in hardness due to the fact that the microsphere components are not contained, the hardness difference between the end point detection window with single hardness and the surrounding polishing layer is large, so that a polished element is easy to produce large scratches and even fragments when passing through the end point detection window, and the product yield is affected. When the hardness of the end point detection window is too low, the window is easy to deform, crack and the like due to mechanical movement in the polishing process. The difference between the maximum Shore hardness and the minimum Shore hardness is regulated to be 0< D1-D2 and less than or equal to 2, so that the overlarge hardness difference between the end point detection window and the polishing layer can be prevented, the polished element is easy to scratch and generate fragments, and the yield of the polished element is reduced.
2. According to the preparation method of the end point detection window, the hardness of the end point detection window can be changed in a gradient manner from the periphery to the center by regulating and controlling the chain extension coefficient of the two mixtures, the hardness of the end point detection window is gradually increased from the edge to the center, the difference value of the hardness of the edge of the end point detection window, which is in contact with the polishing layer, can be ensured to have no obvious change, the deformation in the polishing process caused by the softer end point detection window can be prevented, the defects that the end point detection window does not contain microsphere components, the hardness is higher than that of the polishing layer, and the wafer is scratched, inconsistent in polishing, broken and the like due to the difference of the hardness of the interface of the polishing layer and the end point detection window in the prior art are overcome.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a top view of a polishing pad of example 1 of the present invention;
FIG. 2 is a front view of a polishing pad of example 1 of the present invention;
reference numerals:
1-polishing pad, 2-polishing layer, 3-adhesive layer, 4-buffer layer, 5-endpoint detection window.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
The raw material sources and equipment used in the following examples and comparative examples
Isocyanate terminated prepolymer containing unreacted NCO group the Adiprene prepolymer LF750D produced by Chemtura had an unreacted NCO group content of 8.95% by weight.
Isocyanate terminated prepolymer containing unreacted NCO group the Adiprene prepolymer LF751D produced by Chemtura had an unreacted NCO group content of 9.02% by weight.
Isocyanate terminated prepolymer containing unreacted NCO group the Adiprene prepolymer L325 produced by Chemtura had an unreacted NCO group content of 9.11% by weight.
The curing agent is MOCA, 4' -methylenebis (2-chloroaniline), is used in Jinan Lunan chemical industry, and has the active hydrogen content of 12 percent.
The curing agent is butanediol, the active hydrogen content is 37.8 percent in Shandong Rui Kong chemical industry.
Polishing equipment and polishing conditions Applied Reflexion polishing machine (applied materials Co.) wherein the carrier (corresponding to the polishing head) had a downforce of 0.024MPa and the slurry flow rate of the polishing liquid was 300mL/min. The table rotation speed was 93rpm, and the carrier rotation speed was 87rpm.
Example 1
The embodiment provides a preparation method of an endpoint detection window, which comprises the following steps:
18.4kg of isocyanate-terminated prepolymer containing unreacted NCO groups (LF 750D, NCO 8.95%) and 5.5kg of curing agent (MOCA) were placed in a casting machine head A with a chain extension factor of 0.95. 15.6kg of isocyanate-terminated prepolymer containing unreacted NCO groups (LF 750D, NCO 8.95%) and 5.4kg of curing agent (MOCA) were placed in a casting machine head B with a chain extension factor of 0.82. And (3) the casting machine head B moves along the window die outside source, the machine head A moves along the center of the window die, casting is performed simultaneously until the two machine heads are all discharged and full of the whole die, the die is placed into an 80 ℃ oven for 18 hours, and after being taken out, the die is naturally cooled to room temperature, and an end point detection window is obtained after the die is taken out.
In this embodiment, the center point of the end point detection window has the maximum shore D1, the peripheral edge point of the end point detection window has the minimum shore D2, the difference between D1 and D2 is 0.9D, the maximum shore D1 is 73.2D, and the shore hardness gradually increases along the peripheral to central direction.
The embodiment also provides a polishing pad, the structure of which is shown in fig. 1-2, comprising the end point detection window, and the preparation method of the polishing pad comprises the following steps:
(1) And pouring a mixed solution formed by 31.2g of LF750D, 7.9g of MOCA and 0.52g of Norway expansion microsphere Expancel 551D 80d42 into a polishing layer mould, placing the end point detection window into the polishing layer mould, heating the mould in a 90 ℃ oven for 24 hours after pouring, taking out the mould from the oven, naturally cooling to room temperature, and demoulding to obtain the polishing layer 2 with the end point detection window.
(2) The polishing layer 2 was cut to a thickness of 80mil by a microtome, with the DOW commercial SUBA IV product as buffer layer 4 and the decha PSA as adhesive layer 3. The bottom surfaces of the buffer layer 4 and the polishing layer 2 are roll-pressed by the adhesive layer 3 to form a laminated structure, thereby obtaining the polishing pad 1.
Example 2
The embodiment provides a preparation method of an endpoint detection window, which comprises the following steps:
15.5kg of isocyanate-terminated prepolymer containing unreacted NCO groups (LF 751D, NCO 9.02%) and 1.6kg of curing agent (butanediol) were placed in a casting machine head A with a chain extension of 0.94. 15.8kg of isocyanate-terminated prepolymer containing unreacted NCO groups (LF 751D, NCO 9.02%) and 1.8kg of curing agent (butanediol) were placed in a casting machine head B with a chain extension factor of 0.85. And (3) the casting machine head B moves along the window die outside source, the machine head A moves along the center of the window die, casting is carried out until the two machine heads are all discharged and the whole die is filled, the die is placed into an 80 ℃ oven for 18 hours, the die is naturally cooled to room temperature after being taken out, and a terminal detection window is obtained after the die is taken out.
In this embodiment, the center point of the end point detection window has the maximum shore D1, the peripheral edge point of the end point detection window has the minimum shore D2, the difference between D1 and D2 is 1.2D, the maximum shore D1 is 72.9D, and the shore hardness gradually increases along the peripheral to central direction.
This example also provides a polishing pad prepared in the same manner as example 1 using the endpoint detection window of this example.
Example 3
The embodiment provides a preparation method of an endpoint detection window, which comprises the following steps:
19.3kg of isocyanate-terminated prepolymer (L325, NCO 9.11%) containing unreacted NCO groups and 1.8kg of a curing agent (butanediol) were placed in a casting machine head A, with a chain extension factor of 0.98. 18.7kg of isocyanate-terminated prepolymer (L325, NCO 9.11%) containing unreacted NCO groups and 2.0kg of a curing agent (butanediol) were placed in a casting machine head B, with a chain extension factor of 0.86. And (3) the casting machine head B moves along the window die outside source, the machine head A moves along the center of the window die, casting is carried out until the two machine heads are all discharged and the whole die is filled, the die is placed into an 80 ℃ oven for 18 hours, the die is naturally cooled to room temperature after being taken out, and a terminal detection window is obtained after the die is taken out.
In this embodiment, the center point of the end point detection window has the maximum shore D1, the peripheral edge point of the end point detection window has the minimum shore D2, the difference between D1 and D2 is 1.3D, the maximum shore D1 is 73D, and the shore hardness gradually increases along the peripheral to central direction.
This example also provides a polishing pad prepared in the same manner as example 1 using the endpoint detection window of this example.
Comparative example 1
The comparative example provides a method for preparing an endpoint detection window, comprising the following steps:
36.8kg of isocyanate terminated prepolymer containing unreacted NCO groups (LF 750D, NCO 8.95%) and 11kg of curing agent (MOCA) are placed into a casting machine head to be cast until the whole mold is completely discharged and filled, the mold is placed into an 80 ℃ oven for 18 hours, taken out and naturally cooled to room temperature, and an end point detection window is obtained after the mold is taken out.
The present embodiment is the shore hardness of the endpoint detection window with uniform shore hardness, and the shore hardness is 71.4D.
This comparative example also provides a polishing pad prepared in the same manner as in example 1 using the endpoint detection window of this comparative example.
Comparative example 2
The comparative example provides a method for preparing an endpoint detection window, comprising the following steps:
31.2kg of isocyanate terminated prepolymer (LF 750D, NCO 8.95%) containing unreacted NCO groups and 10.8kg of curing agent (MOCA) are placed into a casting machine head to be cast until the whole mold is completely discharged and filled, the mold is placed into an 80 ℃ oven for 18 hours, taken out and naturally cooled to room temperature, and an end point detection window is obtained after the mold is taken out.
The present embodiment is the shore hardness of the endpoint detection window with uniform shore hardness, and the shore hardness is 73.2D.
This comparative example also provides a polishing pad prepared in the same manner as in example 1 using the endpoint detection window of this comparative example.
Comparative example 3
The comparative example provides a method for preparing an endpoint detection window, comprising the following steps:
18.4kg of isocyanate-terminated prepolymer containing unreacted NCO groups (LF 750D, NCO 8.95%) and 4.3kg of curing agent (MOCA) were placed in a casting machine head A with a chain extension of 1.22. 15.6kg of isocyanate-terminated prepolymer containing unreacted NCO groups (LF 750D, NCO 8.95%) and 6.2kg of curing agent (MOCA) were placed in a casting machine head B with a chain extension factor of 0.71. And (3) the casting machine head B moves along the window die outside source, the machine head A moves along the center of the window die, casting is carried out until the two machine heads are all discharged and the whole die is filled, the die is placed into an 80 ℃ oven for 18 hours, the die is naturally cooled to room temperature after being taken out, and a terminal detection window is obtained after the die is taken out.
The center point of the end point detection window of the comparative example has the maximum Shore hardness D1, the peripheral edge point of the end point detection window has the minimum Shore hardness D2, the difference between D1 and D2 is 3.3D, the maximum Shore hardness D1 is 76.9D, and the Shore hardness gradually increases along the peripheral to central direction.
This comparative example also provides a polishing pad prepared in the same manner as in example 1 using the endpoint detection window of this comparative example.
Comparative example 4
This comparative example provides a method of preparing an endpoint detection window, differing from comparative example 3 in that both the head A and the head B move in opposite directions to comparative example 3.
The center point of the end point detection window of the comparative example has the minimum Shore hardness D1, the peripheral edge point of the end point detection window has the maximum Shore hardness D2, the difference between D2 and D1 is 3.3D, the maximum Shore hardness D2 is 76.9D, and the Shore hardness gradually becomes smaller along the peripheral to central direction.
This comparative example also provides a polishing pad prepared in the same manner as in example 1 using the endpoint detection window of this comparative example.
Test case
The test examples provide the results of performance testing of the endpoint detection windows and polishing pads prepared in the examples and comparative examples, as follows:
The hardness testing method of the end point detection window is used for testing the Shore hardness D by referring to GB/T2411-2008 national standard plastic and hard rubber, indentation hardness (Shore hardness) is measured by using a durometer.
The wafer is used as a polished element, a polishing machine (model is F-REX 300X), D3000 is used as polishing liquid, the flow rate of the polishing liquid is 250ml/min, the polishing time is 60s, the TT/TR rotating speed is 93/87, the pressure is 204/202/203/201/197/191/204/317/318, the non-uniformity ratio (% NUR) is obtained after polishing is finished, and the smaller the non-uniformity ratio, namely the smaller the standard deviation of the removal rate, the closer the polishing rate is on the whole polished surface, and the more uniform the polishing effect is. The polishing pads of each example and comparative example were tested according to the above method to obtain non-uniformity ratios, respectively, and the results are shown in Table 1.
And (3) observing the number of scratches on the polished wafer surface by using a Zeiss optical microscope, and counting the number of scratches with the maximum width of more than 5 mu m, wherein the scratches with the maximum width of less than or equal to 5 mu m are negligible scratches.
Table 1 test results for each of the examples and comparative examples
In the table "/" indicates that the data is not present.
From the results, the hardness of the end point detection window is adjusted to gradually increase from the periphery to the center, and the difference between the maximum Shore D1 and the minimum Shore D2 satisfies that 0< D1-D2 is less than or equal to 2, so that the device to be polished is favorable for reducing the generation of larger scratches when passing through the end point detection window, and the product yield is improved. In addition, the difference between the maximum Shore D1 and the minimum Shore D2 is too large, so that defects are easily generated, and polishing performance such as scratch resistance, polishing uniformity and the like are affected.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
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