CN111599707A - Method for detecting micro-cracks of passivation layer - Google Patents
Method for detecting micro-cracks of passivation layer Download PDFInfo
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- CN111599707A CN111599707A CN202010462604.3A CN202010462604A CN111599707A CN 111599707 A CN111599707 A CN 111599707A CN 202010462604 A CN202010462604 A CN 202010462604A CN 111599707 A CN111599707 A CN 111599707A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
- H01L22/24—Optical enhancement of defects or not directly visible states, e.g. selective electrolytic deposition, bubbles in liquids, light emission, colour change
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for detecting microcracks of a passivation layer, which comprises the steps of immersing a sample to be detected in a corrosion solution, enabling the corrosion solution to enter a metal layer in contact with the microcracks through the microcracks in the passivation layer, corroding the metal layer to form metal corrosion cavities which are relatively large in microcracks and black under an optical microscope, and obtaining the microcracks which cannot be observed due to the fact that the passivation layer is in a transparent state and small in size under the optical microscope by observing the distribution of the metal corrosion cavities. According to the detection method, the corrosion solution can enter all microcracks which are in contact with the metal layer to form the metal corrosion cavity, compared with the existing profile observation technology, the distribution condition of the microcracks in the passivation layer can be integrally reflected, the whole detection process is a chemical corrosion process, new stress is not generated, new microcracks cannot be formed in the passivation layer to interfere the detection result, large and expensive detection equipment is not needed, the detection method is simple, and the detection cost is low.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a method for detecting microcracks of a passivation layer.
Background
The chip passivation layer is a protective layer for protecting the internal circuit structure of the chip from the outside (moisture, corrosive gas, impurities or external force). Microcracks in the passivation layer can cause water, gas, or impurities to enter through the microcracks, corrode or otherwise affect the electrical properties of the metal layer under the protection of the passivation layer, thereby causing chip failure or reduced reliability. The microcracks are not observable under an optical microscope because of their small size, typically on the scale of tens of nanometers or less, and because visible light can pass through the passivation layer.
The main technique for detecting the micro-cracks of the passivation layer at present is to make a section of a sample (the most part of the section is made by a mechanical method or cut by a focused ion beam), and then observe whether the section has the micro-cracks by using a scanning electron microscope. This detection method has the following disadvantages: (1) the microcracks of the section are not enough to reflect the distribution of the microcracks in the passivation layer of the chip, because the microcracks are not uniformly distributed in the passivation layer, and the microcracks of a single section are not enough to reflect the distribution of the microcracks in the passivation layer; (2) stress is generated in the process of manufacturing the section of the sample to be detected by a mechanical method, the passivation layer is made of brittle materials, new microcracks can be caused by the mechanical stress and influence on the appearance of the original microcracks, the section manufactured by adopting focused ion beam cutting is very small in size, the condition of a long-size section is difficult to reflect, and the condition of the whole passivation layer is difficult to reflect; (3) large-scale equipment such as a scanning electron microscope, a focused ion beam cutting device, a wafer cutting device and the like is required, the operation is complex, and the time consumption is long.
Disclosure of Invention
The invention aims to provide a method for detecting microcracks in a passivation layer, which is used for integrally reflecting the distribution condition of the microcracks in the passivation layer.
In order to achieve the above object, the present invention provides a method for detecting microcracks in a passivation layer, comprising:
immersing a sample to be detected in a corrosive solution, wherein the corrosive solution enters a metal layer in contact with the microcracks through the microcracks in the passivation layer, and corroding the metal layer to form a metal corrosion hole; and
observing the distribution of the metal corrosion holes under an optical microscope.
Optionally, the etching solution comprises hydrochloric acid or nitric acid.
Optionally, a surfactant is further added to the etching solution.
Optionally, the etching solution comprises 3% by weight of a surfactant, 8% by weight of hydrochloric acid and 89% by weight of deionized water.
Optionally, before immersing the sample to be detected in the etching solution, the passivation layer is further treated by using a surfactant, so that the capability of the microcrack interface in the passivation layer to be wetted by the etching solution is increased.
Optionally, before the passivation layer is treated with the surfactant, the sample to be detected is further cleaned to remove the contamination in the microcracks and/or on the surface of the passivation layer, so that the microcracks are completely exposed.
Optionally, the cleaning solution for cleaning the sample to be detected includes hydrofluoric acid, nitric acid, and a mixed solution of hydrofluoric acid and nitric acid.
Optionally, the cleaning solution comprises 2% nitric acid, 2% hydrofluoric acid by weight, and 96% deionized water by weight.
Optionally, the method further comprises cleaning the sample to be detected in a first set temperature range, and/or immersing the sample to be detected in an etching solution in a second set temperature range.
Optionally, the first set temperature range and the second set temperature range are both 40 ℃ to 60 ℃.
Optionally, a buffer reagent is further added to the etching solution.
Optionally, the buffering agent comprises an acetic acid solution.
Optionally, the passivation layer includes a silicon oxide layer in contact with the metal layer and a silicon nitride layer on the silicon oxide layer.
Optionally, the material of the metal layer includes aluminum or an aluminum alloy.
In summary, the present invention provides a method for detecting microcracks in a passivation layer, including immersing a sample to be detected in an etching solution, allowing the etching solution to enter a metal layer contacting with the microcracks through the microcracks in the passivation layer, etching the metal layer to form metal corrosion cavities, and observing the distribution of the metal corrosion cavities under an optical microscope to obtain the distribution of the microcracks in the passivation layer. The sample to be detected is wholly immersed into the corrosive solution, and the corrosive solution enters all microcracks which are in contact with the metal layer to form a metal corrosion cavity, so that the distribution condition of the microcracks in the passivation layer can be wholly reflected compared with the existing section observation technology; the whole process of the detection method adopted by the invention is a chemical corrosion process, no new stress is generated, and no new micro-crack is formed in the passivation layer to interfere the detection result; in addition, the detection method provided by the invention only needs a certain proportion of corrosion solution and an optical microscope, does not need a large and expensive scanning electron microscope, focused ion beam cutting equipment, wafer cutting equipment and the like, and is simple and low in detection cost.
Drawings
Fig. 1 is a flowchart of a method for detecting microcracks in a passivation layer according to an embodiment of the present invention;
fig. 2 to fig. 4 are schematic structural diagrams corresponding to corresponding steps in a method for detecting microcracks in a passivation layer according to an embodiment of the present invention;
wherein the reference numerals are:
100-a substrate; 200-a device layer; 300-a metal layer; 400-a passivation layer; 400 a-a silicon oxide layer; 400 b-a silicon nitride layer; 500-microcracking; 600-etching solution; 700-metal corrosion voids.
Detailed Description
The method for detecting microcracks in a passivation layer according to the present invention is further described in detail below with reference to the accompanying drawings and specific examples. The advantages and features of the present invention will become more apparent from the following description and drawings, it being understood, however, that the concepts of the present invention may be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein. The drawings are in simplified form and are not to scale, but are provided for convenience and clarity in describing embodiments of the invention.
The terms "first," "second," and the like in the description are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the invention described herein are, for example, capable of operation in other sequences than described or illustrated herein. Similarly, if the method described herein comprises a series of steps, the order in which these steps are presented herein is not necessarily the only order in which these steps may be performed, and some of the described steps may be omitted and/or some other steps not described herein may be added to the method. Although elements in one drawing may be readily identified as such in other drawings, the present disclosure does not identify each element as being identical to each other in every drawing for clarity of description.
Fig. 1 is a flowchart of a method for detecting microcracks in a passivation layer according to this embodiment, and as shown in fig. 1, the method for detecting microcracks in a passivation layer according to this embodiment includes:
s01: immersing a sample to be detected in a corrosive solution, wherein the corrosive solution enters a metal layer in contact with the microcracks through the microcracks in the passivation layer, and corroding the metal layer to form a metal corrosion hole; and
s02: observing the distribution of the metal corrosion holes under an optical microscope.
Fig. 2 to fig. 4 are schematic structural diagrams corresponding to corresponding steps of the method for detecting microcracks in a passivation layer provided in this embodiment. The method for detecting microcracks in a passivation layer according to the present embodiment will be described in detail below with reference to fig. 1 to 4.
First, step S01 is executed to immerse the sample to be tested in an etching solution, which enters the metal layer contacting with the microcracks through the microcracks in the passivation layer, and etch the metal layer to form metal corrosion cavities.
Specifically, first, a sample to be detected is prepared, and if the sample to be detected is a chip package, a chemical reagent may be used to remove the packaging material around the chip, so as to take out or expose the chip. If the sample to be detected is a wafer, the size of the sample can be made according to the observation requirement, and the size of the sample to be detected is 1cm by 1cm and at least one chip should be included. The sample to be detected is prepared by adopting a traditional sample preparation method for cutting a section, the preparation of the section sample with the length of 10 microns is generally carried out, the time consumption is about one hour, the size of one chip is generally more than 5mm, and the time consumption for preparing the sample to be detected is long. In the embodiment, only chemical reagents are needed to expose the microcracks of the passivation layer of the chip to be detected, so that subsequent corrosive solution enters the metal layer through the microcracks, sample preparation by large-scale equipment such as focused ion beams or wafer cutting equipment is not needed, and the detection time is saved.
As shown in fig. 2, the manufactured sample to be tested includes a substrate 100, a device layer 200 formed on the substrate, a metal layer 300 formed on the device layer 200, and a passivation layer 400 formed on the metal layer 300.
The substrate 100 may be at least one of the following materials: si, Ge, SiGe, SiC, SiGeC, InAs, GaAs, InP or other III/V compound semiconductors, and the substrate may be a multilayer structure or the like of these semiconductor materials or silicon-on-insulator (SOI), silicon-on-insulator (SSOI), silicon-on-insulator-germanium (S-SiGeOI), silicon-on-insulator-germanium (SiGeOI), germanium-on-insulator (GeO), or the like. The device layer 200 includes an interconnection structure formed by depositing a thin film, performing photolithography, etching, ion implantation, etc. on the substrate 100 to form devices such as NMOS and/or PMOS, and dielectric layers and metal layers. The material of the metal layer 300 may include one or more of copper, silver, gold, nickel, tungsten, and the like, for example, the material of the metal layer 300 is aluminum or aluminum alloy. The passivation layer 400 covers the metal layer 300 to protect active devices formed in the device layer 200. In some embodiments, passivation layer 400 is also a sealing layer to prevent moisture from contacting the device. The passivation layer 400 is formed of a nitride, oxide, oxynitride, polymer, or other dielectric material. The passivation layer 400 may be formed by Chemical Vapor Deposition (CVD), Plasma Enhanced Chemical Vapor Deposition (PECVD), spin coating, or the like. In this embodiment, the metal layer is made of copper or copper alloy, and the passivation layer 400 includes a silicon oxide layer 400a in contact with the metal layer 300 and a silicon nitride layer 400b on the silicon oxide layer 400 a. At least one micro-crack 500 is distributed in the passivation layer 400 in contact with the metal layer 300.
Next, the test sample is cleaned to remove contaminants in the microcracks 500 and/or on the surface of the passivation layer 400, leaving the microcracks 500 fully exposed. For example, the sample to be tested may be put into the washing solution for a set time, for example, 1min, and then the sample to be tested may be taken out and dried. The cleaning solution for cleaning the sample to be detected can be a mixed solution of hydrofluoric acid, nitric acid and a mixed solution of hydrofluoric acid and nitric acid. In this embodiment, the cleaning solution includes 2% by weight of nitric acid, 2% by weight of hydrofluoric acid, and 96% by weight of deionized water, where the nitric acid is concentrated nitric acid, the mass fraction of the nitric acid is about 70%, and the mass fraction of the hydrofluoric acid is about 37%. Optionally, the sample to be tested may be washed at the first set temperature range to improve the washing ability of the washing solution. The first predetermined temperature range is 40 ℃ to 60 ℃, for example, 45 ℃, 50 ℃, or 55 ℃. In other embodiments of the present invention, the cleaning solution may also use other chemical reagents, and the temperature range of the cleaning may also be selected according to different cleaning solutions and materials of the passivation layer, which is not limited herein.
Then, the passivation layer 400 is treated by using a surfactant, so that the capability of the microcrack interface in the passivation layer 400 to be wetted by a subsequent etching solution is increased, the surface tension of the microcrack 500 in the passivation layer 400 is changed, and the etching solution smoothly enters the microcrack 500. The surfactant may include a copolymer alcohol of Ethylene Oxide (EO) and Propylene Oxide (PO), although other surface chemistries may be used.
Next, the sample to be tested is immersed in the etching solution 600 for a set time, so that the etching solution 600 enters the metal layer 300 contacting the microcracks 500 through the microcracks 500 in the passivation layer 400, as shown in fig. 3. The etching solution 600 may be hydrochloric acid, nitric acid, or a chemical solution that is corrosive to the metal layer 300 but is not reactive to the passivation layer 400.
It should be noted that the treatment of the passivation layer 400 with the surfactant may be performed before the sample to be detected is immersed in the etching solution 600, or the surfactant may be mixed with the etching solution, that is, the surfactant is added to the etching solution, and the surface activation of the passivation layer 400 and the etching of the metal layer 300 are performed in the same step. Specifically, in this embodiment, the etching solution includes 3% by weight of a surfactant, 8% by weight of hydrochloric acid, and 89% by weight of deionized water, where the hydrochloric acid is concentrated hydrochloric acid (mass fraction is about 37%), the hydrochloric acid may also be replaced by dilute nitric acid, and the deionized water may adjust the concentrations of the above chemical substances, control the reaction rate, or of course, add an H + buffer such as acetic acid to the deionized water, and adjust the reaction rate. In other embodiments of the present invention, the ratio of the surface active agent, the hydrochloric acid, and the deionized water may be adjusted according to actual needs, and other etching solutions may be used.
Optionally, the sample to be detected may be immersed in the etching solution 600 within the second set temperature range, so that the etching solution 600 can more easily enter the crack 500, and the corrosion of the metal layer by the etching solution is also promoted. For example, a heating stage may be used to heat the etching solution 600 so that the temperature of the etching solution 600 is within a second predetermined temperature range. The second set temperature range may be the same as the first set temperature range, or may be adjusted accordingly according to actual needs.
Next, as shown in fig. 3 and 4, after the sample to be tested is immersed in the etching solution 600 for a set time, for example, 3min, the etching solution 600 enters the metal layer 300 contacting with the microcracks 500 through the microcracks 500 in the passivation layer 400, and the metal layer 300 is etched to form metal etching holes 700 with a size suitable for easy observation.
Next, step S02 is performed, and as shown in fig. 4, the distribution of the metal corrosion holes 700 is observed under an optical microscope. And processing the sample to be detected soaked in the corrosion solution 600, and then transferring the sample to be detected to an optical microscope for observation. Since visible light can penetrate through the passivation layer 400, the microcracks 500 in the passivation layer 400 cannot be observed under an optical microscope, but the metal corrosion holes 700 generated by corrosion are larger than the microcracks 500 in the passivation layer 400, and appear black under the optical microscope, so that the metal corrosion holes 700 are distributed in a one-to-one correspondence with the distribution of the microcracks 500 in the passivation layer 400, and therefore, the distribution of the microcracks 500 in the passivation layer 400 can be estimated by observing the distribution of the metal corrosion holes 700 under the optical microscope.
In summary, the present invention provides a method for detecting microcracks in a passivation layer, including immersing a sample to be detected in an etching solution, allowing the etching solution to enter a metal layer contacting with the microcracks through the microcracks in the passivation layer, etching the metal layer to form metal corrosion cavities, and observing the distribution of the metal corrosion cavities under an optical microscope to obtain the distribution of the microcracks in the passivation layer. The sample to be detected is wholly immersed into the corrosive solution, and the corrosive solution enters all microcracks which are in contact with the metal layer to form a metal corrosion cavity, so that the distribution condition of the microcracks in the passivation layer can be wholly reflected compared with the existing section observation technology; the whole process of the detection method adopted by the invention is a chemical corrosion process, no new stress is generated, and no new micro-crack is formed in the passivation layer to interfere the detection result; in addition, the detection method provided by the invention only needs a certain proportion of corrosion solution and an optical microscope, does not need a large and expensive scanning electron microscope, focused ion beam cutting equipment, wafer cutting equipment and the like, and is simple and low in detection cost.
The above description is only for the purpose of describing the preferred embodiments of the present invention, and is not intended to limit the scope of the present invention, and any variations and modifications made by those skilled in the art based on the above disclosure are within the scope of the appended claims.
Claims (14)
1. A method for detecting microcracks in a passivation layer, comprising:
immersing a sample to be detected in a corrosive solution, wherein the corrosive solution enters a metal layer in contact with the microcracks through the microcracks in the passivation layer, and corroding the metal layer to form a metal corrosion hole; and
observing the distribution of the metal corrosion holes under an optical microscope.
2. The method for detecting microcracks in a passivation layer according to claim 1, wherein the etching solution comprises hydrochloric acid or nitric acid.
3. The method for detecting microcracks in a passivation layer according to claim 2, wherein a surfactant is further added to the etching solution.
4. The method for detecting microcracks in a passivation layer according to claim 3, wherein the etching solution comprises 3% by weight of surfactant, 8% by weight of hydrochloric acid and 89% by weight of deionized water.
5. The method for detecting microcracks in a passivation layer according to claim 1, wherein before immersing the sample to be detected in the etching solution, the method further comprises treating the passivation layer with a surfactant.
6. The method for detecting microcracks in a passivation layer according to claim 5, wherein before the passivation layer is treated by the surfactant, the method further comprises cleaning the sample to be detected to remove contamination in the microcracks and/or on the surface of the passivation layer, so that the microcracks are completely exposed.
7. The method for detecting micro-cracks of the passivation layer according to claim 6, wherein the cleaning solution used for cleaning the sample to be detected comprises hydrofluoric acid, nitric acid and a mixed solution of hydrofluoric acid and nitric acid.
8. The method for detecting microcracks in a passivation layer according to claim 7, wherein the cleaning solution comprises 2% nitric acid, 2% hydrofluoric acid and 96% deionized water by weight.
9. The method for detecting microcracks in a passivation layer according to claim 8, further comprising cleaning the sample to be detected in a first set temperature range and/or immersing the sample to be detected in an etching solution in a second set temperature range.
10. The method for detecting microcracks in a passivation layer according to claim 9, wherein the first set temperature range and the second set temperature range are both 40 ℃ to 60 ℃.
11. The method for detecting microcracks in a passivation layer according to any one of claims 1 to 10, wherein a buffer reagent is further added to the etching solution.
12. The method for detecting microcracks in a passivation layer according to claim 11, wherein the buffer reagent comprises an acetic acid solution.
13. The method for detecting microcracks in a passivation layer according to any one of claims 1 to 10, wherein the passivation layer comprises a silicon oxide layer in contact with the metal layer and a silicon nitride layer on the silicon oxide layer.
14. Method for the detection of microcracks in a passivation layer according to any of claims 1 to 10, characterized in that the material of the metal layer comprises aluminum or an aluminum alloy.
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| CN202010462604.3A CN111599707A (en) | 2020-05-27 | 2020-05-27 | Method for detecting micro-cracks of passivation layer |
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| CN202010462604.3A CN111599707A (en) | 2020-05-27 | 2020-05-27 | Method for detecting micro-cracks of passivation layer |
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| CN202010462604.3A Pending CN111599707A (en) | 2020-05-27 | 2020-05-27 | Method for detecting micro-cracks of passivation layer |
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Cited By (4)
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| CN112185839A (en) * | 2020-10-27 | 2021-01-05 | 上海华虹宏力半导体制造有限公司 | Passivation layer test structure |
| CN112259455A (en) * | 2020-10-19 | 2021-01-22 | 扬州扬杰电子科技股份有限公司 | Method for improving metal residue of Ag surface product with passivation layer structure |
| CN113097088A (en) * | 2021-03-29 | 2021-07-09 | 工业和信息化部电子第五研究所华东分所 | Method for detecting pin hole defects of chip |
| CN116274562A (en) * | 2023-03-06 | 2023-06-23 | 佛山市顺德区华峻杨铜业有限公司 | Stamping process for copper product processing |
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