TW201610409A - Method for preparing transmission electron microscope sample - Google Patents

Abstract

A method for preparing a transmission electron microscope (TEM) sample including following steps is provided. A first thinning treatment is performed to an observation object to form a TEM sample having a thickness resistant to chemical treatment in a predetermined observation region of the observation object. A chemical treatment is performed to the TEM sample at room temperature. A second thinning treatment is performed to the TEM sample which has undergone the chemical treatment, so that the TEM sample has a thickness for observation by a TEM. The TEM sample is removed from the observation object.

Description

Method for preparing transmissive electron microscope test piece

The invention relates to a preparation method of a test piece, and in particular to a preparation method of a transmission electron microscope (TEM) test piece.

In the semiconductor process, when the process material and the defect material have the same crystal structure composed of different elements, it is sometimes difficult to distinguish the interface in the transmission electron microscope observation, and the existence position of the defect cannot be clearly judged.

Therefore, at present, in the process of preparing a transmissive electron microscope test piece, a chemical treatment technique is added, which can make the thickness of the test piece of different materials after etching to be different and easily distinguish the defect in the transmission electron microscope. The location of existence.

The preparation methods of common transmission electron microscope test strips can be mainly classified into the following two methods. The polishing method using the polishing cloth is to directly grind the test piece to a thickness for observation by a transmission electron microscope, and then chemically treat the test piece. However, since the polished test piece is very thin, it must be controlled by chemical treatment. The temperature is used to control the etch rate to avoid damage to the test piece. In addition, grinding methods using abrasive cloths do not provide fixed-point micro-area defect analysis.

Another method for preparing an electron microscope test piece is to perform a chemical treatment on a test piece by using a focused ion beam to prepare a transmission electron microscope test piece for fixed-point micro-area analysis. Also, since the thickness of the observation area of the test piece after the focused ion beam treatment is very thin, it is necessary to control the etching rate by controlling the temperature of the chemical treatment to avoid damage of the test piece.

The invention provides a preparation method of a transmission electron microscope test piece, which can chemically treat a transmission electron microscope test piece at room temperature without causing damage to the transmission electron microscope test piece.

The invention provides a preparation method of a transmission electron microscope test piece, which comprises the following steps. The observation object is subjected to a first thinning treatment, and a transmission electron microscope test piece having a chemically resistant thickness is formed in a predetermined observation area of the observation object. The transmission electron microscopy test piece was chemically treated at room temperature. The chemically treated transmission electron microscope test piece was subjected to a second thinning treatment so that the transmission electron microscope test piece had a thickness for observation by a transmission electron microscope. A transmission electron microscope test piece was taken out from the observation object.

According to an embodiment of the present invention, in the above method for producing a transmission electron microscope test strip, the first thinning treatment is performed using, for example, a focused ion beam.

According to an embodiment of the present invention, in the method for preparing a transmission electron microscope test piece, the first thinning treatment may be a single-pass thinning treatment or a multi-pass thinning treatment.

According to an embodiment of the present invention, in the preparation method of the transmissive electron microscope test piece, the multi-pass thinning process includes first roughening and thinning the observation object, and then thinning the observation object. deal with.

According to an embodiment of the present invention, in the preparation method of the above-mentioned transmission electron microscope test piece, the chemical treatment is, for example, a dopant-solution dip or an oxide etching solution immersion treatment (oxide- Etching solution dip).

According to an embodiment of the present invention, in the above method for producing a transmission electron microscope test strip, the second thinning treatment includes using a focused ion beam.

According to an embodiment of the present invention, in the method for preparing a transmission electron microscope test piece, after performing the chemical treatment, the method further comprises performing a water-washing treatment on the transmission electron microscope test piece.

According to an embodiment of the present invention, in the preparation method of the transmissive electron microscope test piece, after performing the bubble water cleaning process, the transmission electron drying test piece is further subjected to a heat drying process.

According to an embodiment of the present invention, in the method for preparing a transmission electron microscope test piece, the method for taking out the transmission electron microscope test piece from the observation object is, for example, performing a single-pass cutting process or a multi-pass cutting. Process.

Transmissive electron microscopy as described above in accordance with an embodiment of the present invention In the preparation method of the mirror test piece, the multi-pass cutting process includes the following steps. After the chemical treatment, the predetermined observation of the observation object is U-shaped, and the transmission electron microscope test piece has not been cut from the observation object, and is formed between the transmission electron microscope test piece and the observation object. Connection. After the second thinning treatment, the joint portion was cut, and the transmission electron microscope test piece was taken out from the observation object.

Based on the above, in the preparation method of the transmission electron microscope test piece proposed by the present invention, since the transmission electron microscope test piece after the first thinning treatment of the observation object has a chemically resistant thickness, it has a comparative Good test strip strength. Therefore, even if the transmission electron microscopy test piece is chemically treated at room temperature, it will not cause damage to the transmission electron microscope test piece. In addition, since the method for preparing the transmission electron microscope test piece proposed by the present invention is to form a transmission electron microscope test piece in a predetermined observation area, it can be used for the analysis of the fixed-point micro-area defect.

The above described features and advantages of the invention will be apparent from the following description.

100‧‧‧ Observations

102‧‧‧Predetermined viewing area

104‧‧‧Transmission electron microscope test strips

106‧‧‧ Groove

108‧‧‧Connecting Department

200‧‧‧ test tube

202‧‧‧Chemicals

S100, S102, S104, S110, S120, S130, S140, S150, S160‧‧ ‧ step label

T1, T2, T3‧‧‧ thickness

FIG. 1 is a flow chart showing the preparation of a transmission electron microscope test piece according to an embodiment of the present invention.

2A to 2C are top views of the observation target and the transmission electron microscope test piece after performing the thinning process of step S102, step S104, and step S150 in Fig. 1, respectively.

Fig. 3 is a schematic view showing a state in which the chemical treatment of step S110 in Fig. 1 is performed, and Fig. 3 is drawn along the line I-I' in Fig. 2B.

4A and 4B are schematic views showing the cutting process of steps S140 and S160 in Fig. 1, respectively, and Figs. 4A and 4B are drawn along the line II-II' in Figs. 2B and 2C, respectively.

FIG. 1 is a flow chart showing the preparation of a transmission electron microscope test piece according to an embodiment of the present invention. 2A to 2C are top views of the observation target and the transmission electron microscope test piece after performing the thinning process of step S102, step S104, and step S150 in Fig. 1, respectively. Fig. 3 is a schematic view showing a state in which the chemical treatment of step S110 in Fig. 1 is performed, and Fig. 3 is drawn along the line I-I' in Fig. 2B. 4A and 4B are schematic views showing the cutting process of steps S140 and S160 in Fig. 1, respectively, and Figs. 4A and 4B are drawn along the line II-II' in Figs. 2B and 2C, respectively.

Referring to FIG. 1 , FIG. 2A and FIG. 2B simultaneously, first, step S100 is performed to perform the first thinning process on the observation object 100, and the chemically treated thickness T2 is formed in the predetermined observation area 102 of the observation object 100. Transmissive electron microscope test strip 104. At the same time, grooves 106 may be formed on both sides of the transmission electron microscope test piece 104. The observation object 100 is, for example, a semiconductor wafer. The predetermined observation area 102 is, for example, a metal oxide semiconductor (MOS) transistor region. The first thinning process is performed, for example, using a focused ion beam. Chemically resistant thickness T2 It is 0.35 micrometers to 0.5 micrometers, but the invention is not limited thereto. In the present embodiment, the chemically resistant thickness T2 is exemplified by 0.35 μm.

In step S100, the first thinning process is described by taking a multi-pass thinning process as an example. The multi-pass process thinning process includes the following steps. First, in step S102, a coarse thinning process is performed on the observation target 100 (please refer to FIG. 2A). The thinning treatment is performed, for example, with a focused ion beam of more than 300 pA. At this time, the thickness T1 of the transmission electron microscope test piece 104 is, for example, 0.5 μm to 1.0 μm, but the invention is not limited thereto. In the present embodiment, the thickness T1 is described by taking 0.5 μm as an example.

Next, in step S104, the observation target 100 is subjected to fine thinning processing (please refer to FIG. 2B). The thinning process can cut off the portion damaged by the high-energy focused ion beam in the roughening process. The thinning treatment is performed, for example, with a focused ion beam of less than 100 pA. At this time, although the thickness T2 of the transmission electron microscope test piece 104 is smaller than the thickness T1, the thickness T2 is maintained to a thickness sufficient for chemical resistance, so that the transmission electron microscope test piece 104 can have sufficient test piece strength to prevent Damage caused by chemical treatment. As described above, the chemically resistant thickness T2 in the present embodiment is described by taking 0.35 μm as an example.

In this embodiment, although the first thinning process is described by taking a multi-pass thinning process as an example, the present invention is not limited thereto. In other embodiments, the first thinning process may also form a transmissive electron microscope test strip 104 having a chemically resistant thickness T2 directly in the predetermined viewing zone 102 using a single pass process thinning process.

Then, referring to FIG. 1 and FIG. 3 simultaneously, proceeding to step S110 at room temperature The transmission electron microscope test strip 104 is chemically treated. The chemical treatment is, for example, a dopant solution immersion treatment or an oxide etching solution immersion treatment, but the invention is not limited thereto. Those skilled in the art can chemically treat the transmission electron microscope test strip 104 by selecting the desired chemical agent according to the component material to be observed and analyzed. For example, the test tube 200 can be used to drop the chemical agent 202 into the recess 106, and the chemical agent 202 is brought into contact with the transmission electron microscope test strip 104 for chemical treatment.

Next, referring to FIG. 1, the step S120 may be selectively performed to perform a water-washing treatment on the transmission electron microscope test piece 104 to remove the chemical on the transmission electron microscope test piece 104.

Thereafter, step S130 is selectively performed, and the transmission electron microscope test piece 104 is subjected to a heat drying process to remove water stains.

Furthermore, referring to FIG. 1 and FIG. 4A simultaneously, step S140 is performed to perform U-cut on the predetermined observation area 102 of the observation target 100. At this time, the transmission electron microscope test piece 104 has not been cut from the observation object 100, but A connection portion 108 is formed between the transmission electron microscope test piece 104 and the observation object 100. U-cuts are performed, for example, using a focused ion beam. When a focused ion beam is used for U-cut, the current of the focused ion beam is, for example, 800 to 1200 pA.

Then, referring to FIG. 1 and FIG. 2C, step S150 is performed to perform a second thinning process on the chemically-treated transmission electron microscope test piece 104, so that the transmission electron microscope test piece 104 has a transmissive type. The thickness T3 observed by an electron microscope. In addition, the second thinning treatment can also remove the residue remaining during the chemical treatment. The product is formed to prevent the area to be analyzed from being obscured by the remaining product. The second thinning process is performed, for example, using a focused ion beam. The second thinning process is performed, for example, with a focused ion beam of less than 100 pA. The thickness T3 for observation by a transmission electron microscope is, for example, 0.1 μm to 0.2 μm, but the invention is not limited thereto. In the present embodiment, the thickness T3 for observation by a transmission electron microscope is described by taking 0.15 μm as an example.

Subsequently, referring to FIG. 1 , FIG. 4A and FIG. 4B simultaneously, step S160 is performed to take out the transmission electron microscope test piece 104 from the observation object 100. The method of taking out the transmission electron microscope test piece 104 is, for example, cutting the connection portion 108, and taking out the transmission electron microscope test piece 104 from the observation object 100. The method of cutting the connecting portion 108 is performed, for example, using a focused ion beam. When the focused ion beam is used to cut the connection 108, the current range of the focused ion beam is, for example, less than 100 pA. Further, when the transmission electron microscopy test piece 104 is prepared using the focused ions, the transmission electron microscope test piece may be taken out by an ex situ lift-out method or an in situ lift-out method. 104.

In this embodiment, the transmissive electron microscope test strip 104 is taken out by a multi-pass cutting process, so that the contaminant produced by the U-cut of step S140 can be tested from the transmission electron microscope by the second thinning process of step S150. On-chip 104 is removed. Further, since the transmissive electron microscope test piece 104 has been U-cut first in step S140, when the transmission electron microscope test piece 104 is taken out from the observation target 100 in step S160, the U-shaped test piece 104 can be greatly reduced. The amount of contaminants produced by the cutting process of step S160.

In this embodiment, although the transmission electron microscope test strip 104 is taken out by using a multi-pass cutting process as an example, the present invention is not limited thereto. In other embodiments, the transmissive electron microscope test strip 104 can also be removed using a single pass cutting process. That is, in the case where the amount of the contaminant generated in the single-pass cutting process is within an allowable range, the U-cut of step S140 may not be performed, and after the second thinning process of step S150 is performed, directly in the step The transmission electron microscope test piece 104 is cut out from the observation object 100 in S160.

According to the above embodiment, in the method of manufacturing the transmission electron microscope test piece 104 of the above embodiment, the transmission electron microscope test piece 104 after the first thinning treatment of the observation object 100 has chemical resistance treatment. The thickness is T2, so it has better test piece strength. Therefore, even if the transmission electron microscope test piece 104 is chemically treated at room temperature, the transmission electron microscope test piece 104 is not damaged. Further, since the transmission electron microscope test strip 104 of the above embodiment is prepared by forming the transmission electron microscope test piece 104 in the predetermined observation area 102, it can be used for the fixed-point micro-area defect analysis.

In summary, the above embodiment has at least the following features. The preparation method of the transmission electron microscope test piece of the above embodiment can chemically treat the transmission electron microscope test piece at room temperature without causing damage to the transmission electron microscope test piece. Further, the preparation method of the transmission electron microscope test piece of the above embodiment can be used for the analysis of the fixed-point micro-region defect.

Although the present invention has been disclosed in the above embodiments, it is not intended to limit the invention, and any one of ordinary skill in the art without departing from the invention. In the spirit and scope, the scope of protection of the present invention is subject to the definition of the appended patent application.

S100, S102, S104, S110, S120, S130, S140, S150, S160‧‧ ‧ step label

Claims (10)

A method for preparing a transmission electron microscope test piece, comprising: performing a first thinning treatment on an observation object, and forming a transmissive type having a chemically resistant thickness in a predetermined observation area of the observation object Electron microscopy test piece; chemically treating the transmissive electron microscope test piece at room temperature; performing a second thinning treatment on the chemically processed the transmission electron microscope test piece to make the transmissive type The electron microscope test piece has a thickness for observation by a transmission electron microscope; and the transmission electron microscope test piece is taken out from the observation object. The method for producing a transmission electron microscope test piece according to claim 1, wherein the first thinning treatment comprises performing using a focused ion beam. The method for preparing a transmission electron microscope test piece according to claim 1, wherein the first thinning treatment comprises a single-pass thinning treatment or a multi-pass thinning treatment. The method for preparing a transmission electron microscope test piece according to claim 3, wherein the multi-channel thinning treatment comprises first roughening and thinning the observation object, and then thinning the observation object. deal with. The method for preparing a transmission electron microscope test piece according to claim 1, wherein the chemical treatment comprises a dopant solution immersion treatment or an oxide etching solution immersion treatment. The production of a transmission electron microscope test piece as described in claim 1 A method of preparing, wherein the second thinning process comprises using a focused ion beam. The method for preparing a transmission electron microscope test piece according to claim 1, wherein after the chemical treatment, the transmission electron microscopy test piece is subjected to a water soaking treatment. The method for preparing a transmission electron microscope test piece according to claim 7, wherein after performing the water washing treatment, the transmission electron drying test piece is further subjected to a heating and drying process. The method for preparing a transmission electron microscope test piece according to claim 1, wherein the method for taking out the transmission electron microscope test piece from the observation object comprises performing a single cutting process or a multi-pass cutting Process. The method for preparing a transmission electron microscope test piece according to claim 9, wherein the multi-pass cutting process comprises: performing U-cutting on the predetermined observation area of the observation object after performing the chemical treatment, At this time, the transmission electron microscope test piece has not been cut out from the observation object, and a connection portion is formed between the transmission electron microscope test piece and the observation object; and after the second thinning process is performed, The connection portion was cut, and the transmission electron microscope test piece was taken out from the observation object.