CN103308365A - Method for preparing triethylenemelamine (TEM) sample - Google Patents
Method for preparing triethylenemelamine (TEM) sample Download PDFInfo
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- CN103308365A CN103308365A CN2013102629085A CN201310262908A CN103308365A CN 103308365 A CN103308365 A CN 103308365A CN 2013102629085 A CN2013102629085 A CN 2013102629085A CN 201310262908 A CN201310262908 A CN 201310262908A CN 103308365 A CN103308365 A CN 103308365A
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- 238000000034 method Methods 0.000 title abstract description 10
- IUCJMVBFZDHPDX-UHFFFAOYSA-N tretamine Chemical compound C1CN1C1=NC(N2CC2)=NC(N2CC2)=N1 IUCJMVBFZDHPDX-UHFFFAOYSA-N 0.000 title abstract 8
- 229950001353 tretamine Drugs 0.000 title abstract 8
- 238000002360 preparation method Methods 0.000 claims abstract description 56
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000004458 analytical method Methods 0.000 claims abstract description 16
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 16
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 238000010894 electron beam technology Methods 0.000 claims description 8
- 238000010884 ion-beam technique Methods 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 208000027418 Wounds and injury Diseases 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000006378 damage Effects 0.000 claims description 3
- 208000014674 injury Diseases 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000012549 training Methods 0.000 abstract description 3
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000000452 restraining effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a triethylenemelamine (TEM) sample. The method comprises the following steps of: S1, setting a sample manufacturing scheme according to a test demand; S2, thinning the sample according to the sample manufacturing scheme; S3, performing U-shaped cutting on the bottom of the thinned sample; S4, rotating the sample subjected to the U-shaped cutting by 90 degrees; S5, depositing electronic bundle platinum and ionic bundle platinum which serve as protection layers on the surface of the sample; S6, cutting the sample to a target place for observation and analysis; S7, optimizing the sample manufacturing scheme according to an observation and analysis result; and S8, repeating the steps from S2-S7 until the manufactured sample meets a requirement. According to the method for preparing the TEM sample, the TEM sample prepared according to a preset scheme can be analyzed quickly and conveniently, so that respective conditions such as the thickness, the uniformity and the pollution degree of the sample can be learned about; the sample manufacturing scheme can be adjusted in an auxiliary manner; great significance is realized for preparation of the TEM sample with a novel structure or training of workers for preparing the novel TEM sample; the method is high in generalization performance.
Description
Technical field
The present invention relates to the semiconductor samples preparing technical field, relate in particular to a kind of preparation method of TEM sample.
Background technology
Along with technique constantly develops toward smaller szie, TEM has replaced SEM becomes topmost semiconductor Physical Property Analysis instrument.Traditional TEM method for making sample comprises: a, dig pit before and after the target area, described sample is thinned to suitable thickness; B, described sample is carried out U-shaped cut, and described TEM sample area is separated from sample to be cut; C, with the sucking-off of described TEM sample and place copper mesh, deliver to described TEM and observe.
See also Figure 14～Figure 16, the quality of described TEM sample preparation has all directly affected the observation effect of TEM such as thickness size, thickness evenness, sample contamination etc.Figure 14 shows that the too thin decrystallized collection of illustrative plates of described silicon-based substrate that causes of sample.Figure 15 shows that too thick copper and the interface, restraining barrier of causing of sample do not know collection of illustrative plates.Figure 16 shows that the sample U-shaped was cut causes ion sputtering to pollute collection of illustrative plates for a long time.
So, in traditional TEM sample making course, thickness of sample and inhomogeneity judgement being relied on fully analyst's personal experience, subjectivity is strong, poor repeatability.Especially, for new sample structure, or new sample preparation personnel need to prepare the TEM sample difficulty that meets the demands larger, efficient is excessively low, can not satisfy the need of production.
Therefore for the problem that prior art exists, this case designer relies on the industry experience for many years of being engaged in, the active research improvement is so there has been the preparation method of a kind of TEM sample of the present invention.
Summary of the invention
The present invention be directed in the prior art, the preparation method of traditional TEM sample relies on analyst's personal experience fully, subjectivity is strong, poor repeatability, and for new sample structure, or new sample preparation personnel need to prepare the TEM sample difficulty that meets the demands larger, efficient is excessively low, and the defectives such as need that can not satisfy production provide a kind of preparation method of TEM sample.
For realizing the present invention's purpose, the invention provides a kind of preparation method of TEM sample, the preparation method of described TEM sample comprises:
Execution in step S1: according to needing of test, set the sample preparation scheme;
Execution in step S2: according to described sample preparation scheme with described sample attenuate;
Execution in step S3: U-shaped is carried out in the bottom of the sample behind the described attenuate cut;
Execution in step S4: with 90 ° of the described rotary samples of cutting through U-shaped;
Execution in step S5: at electron beam platinum and the ion beam platinum of described sample surfaces deposition as protective seam;
Execution in step S6: cut to the target place and carry out observation and analysis;
Execution in step S7: according to the described sample preparation scheme of described observation and analysis result optimizing;
Execution in step S8: repeat implementation step S2～S7, until made samples met requirement.
Alternatively, selected TEM sample area in the described sample preparation scheme.
Alternatively, described sample attenuate is namely formed depression in the both sides of described TEM sample area, described sample is thinned to preset thickness.
Alternatively, described TEM sample is polycrystalline structure (Poly).
Alternatively, described observation and analysis is that U-shaped is cut degree of injury, cutter position, gate oxygen structure, silicon substrate structure, polycrystalline structure, electron beam platinum, ion beam platinum are stopped in front and back, and thickness of sample to be revised and homogeneity one of them or its combination of characterizing.
Alternatively, the thickness of described TEM sample is 90～100nm.
In sum, the preparation method of TEM sample of the present invention, can analyze the TEM sample of preparing according to predetermined scheme quickly and easily, the each side situations such as the thickness of understanding sample, homogeneity, pollution level, the auxiliary sample preparation scheme of adjusting, the TEM sample preparation of new construction or new TEM sample preparation personnel's training are had great help, and generalization is strong.
Description of drawings
Figure 1 shows that the preparation method's of TEM sample of the present invention process flow diagram;
Fig. 2 (a)～Fig. 5 (b) is depicted as the preparation method's of TEM sample of the present invention interim structural representation;
Fig. 6～Figure 13 shows that interim structural representation of the TEM sample preparation of polycrystalline structure (Poly);
Figure 14 shows that the too thin decrystallized collection of illustrative plates of described silicon-based substrate that causes of sample;
Figure 15 shows that too thick copper and the interface, restraining barrier of causing of sample do not know collection of illustrative plates;
Figure 16 shows that the sample U-shaped was cut causes ion sputtering to pollute collection of illustrative plates for a long time.
Embodiment
By the technology contents, the structural attitude that describe the invention in detail, reached purpose and effect, below in conjunction with embodiment and cooperate accompanying drawing to be described in detail.
See also Fig. 1, Figure 1 shows that the preparation method's of TEM sample of the present invention process flow diagram.The preparation method of described TEM sample comprises:
Execution in step S1: according to needing of test, set the sample preparation scheme;
Execution in step S2: according to described sample preparation scheme with described sample attenuate;
Execution in step S3: U-shaped is carried out in the bottom of the sample behind the described attenuate cut;
Execution in step S4: with 90 ° of the described rotary samples of cutting through U-shaped;
Execution in step S5: at electron beam Pt and the ion beam Pt of described sample surfaces deposition as protective seam;
Execution in step S6: cut to the target place and carry out observation and analysis;
Execution in step S7: according to the described sample preparation scheme of described observation and analysis result optimizing;
Execution in step S8: repeat implementation step S2～S7, until made samples met requirement.
See also Fig. 2 (a)～Fig. 5 (b), and in conjunction with consulting Fig. 1, Fig. 2 (a)～Fig. 5 (b) is depicted as the preparation method's of TEM sample of the present invention interim structural representation.The preparation method of described TEM sample comprises:
Execution in step S1: according to needing of test, set the sample preparation scheme, and in described sample preparation scheme, select TEM sample area 11;
Execution in step S2: according to TEM sample area 11 selected in the described sample preparation scheme, with described sample 10 attenuates; Particularly, described sample 10 attenuates are namely formed depression 12 in the both sides of described TEM sample area 11, described sample 10 is thinned to preset thickness;
Execution in step S3: U-shaped is carried out in the bottom 13 of the sample 10 behind the described attenuate cut;
Execution in step S4: with described sample 10 half-twists of cutting through U-shaped;
Execution in step S5: at the surface deposition of described sample 10 electron beam platinum 14 and the ion beam platinum 15 as protective seam;
Execution in step S6: cut to the target area that 16 places carry out observation and analysis;
Execution in step S7: according to the described sample preparation scheme of described observation and analysis result optimizing;
Execution in step S8: repeat implementation step S2～S7, until made sample 10 meets the requirements.
In order to set forth more intuitively the preparation method of TEM sample of the present invention, nonrestrictive enumerating, the TEM sample preparation of polycrystalline structure (Poly) is set forth as example in the existing processing procedure product.
See also Fig. 6～Figure 13, Fig. 6～Figure 13 shows that interim structural representation of the TEM sample preparation of polycrystalline structure (Poly).The TEM sample preparation methods of described polycrystalline structure (Poly) comprising:
Execution in step S1: according to needing of test, set the sample preparation scheme, and in described sample preparation scheme, select TEM sample area 11; Particularly, sample 10a described to be revised is blocked up, according to test request, needs the thickness of sample 10a described to be revised is reduced;
Execution in step S2: according to TEM sample area 11 selected in the described sample preparation scheme, with sample 10a attenuate described to be revised; Particularly, sample 10a attenuate described to be revised is namely formed depression 12 in the both sides of described TEM sample area 11, sample 10a described to be revised is thinned to preset thickness;
Execution in step S3: U-shaped is carried out in the bottom 13 of the sample 10a to be revised behind the described attenuate cut;
Execution in step S4: with the described sample 10a half-twist to be revised of cutting through U-shaped;
Execution in step S5: at the surface deposition of sample 10a described to be revised electron beam platinum 14 and the ion beam platinum 15 as protective seam;
Execution in step S6: cut to the target area that 16 places carry out observation and analysis; Described observation and analysis includes but not limited to that U-shaped is cut degree of injury 161, cutter position 162, gate oxygen structure 163, silicon substrate structure 164, polycrystalline structure 165, electron beam platinum 14, ion beam platinum 15 are stopped in front and back, and sample 10a thickness to be revised and homogeneity sign 166 etc.
Execution in step S7: according to the described sample preparation scheme of described observation and analysis result optimizing; Particularly, the thickness of sample 10a described to be revised is between 113.4～124nm, and test to need the thickness optimum be 90～100nm, therefore need to proceed attenuate to sample 10a described to be revised.
Execution in step S8: repeat implementation step S2～S7, until made sample to be revised 10 meets the requirements, namely finish the preparation of described TEM sample 10b.
In sum, the preparation method of TEM sample of the present invention, can analyze the TEM sample of preparing according to predetermined scheme quickly and easily, the each side situations such as the thickness of understanding sample, homogeneity, pollution level, the auxiliary sample preparation scheme of adjusting, the TEM sample preparation of new construction or new TEM sample preparation personnel's training are had great help, and generalization is strong.
Those skilled in the art all should be appreciated that, in the situation that do not break away from the spirit or scope of the present invention, can carry out various modifications and variations to the present invention.Thereby, if when any modification or modification fall in the protection domain of appended claims and equivalent, think that the present invention contains these modifications and modification.
Claims (6)
1. the preparation method of a TEM sample is characterized in that, the preparation method of described TEM sample comprises:
Execution in step S1: according to needing of test, set the sample preparation scheme;
Execution in step S2: according to described sample preparation scheme with described sample attenuate;
Execution in step S3: U-shaped is carried out in the bottom of the sample behind the described attenuate cut;
Execution in step S4: with 90 ° of the described rotary samples of cutting through U-shaped;
Execution in step S5: at electron beam platinum and the ion beam platinum of described sample surfaces deposition as protective seam;
Execution in step S6: cut to the target place and carry out observation and analysis;
Execution in step S7: according to the described sample preparation scheme of described observation and analysis result optimizing;
Execution in step S8: repeat implementation step S2～S7, until made samples met requirement.
2. the preparation method of TEM sample as claimed in claim 1 is characterized in that, selected TEM sample area in the described sample preparation scheme.
3. the preparation method of TEM sample as claimed in claim 1 is characterized in that, described sample attenuate is namely formed depression in the both sides of described TEM sample area, and described sample is thinned to preset thickness.
4. the preparation method of TEM sample as claimed in claim 1 is characterized in that, described TEM sample is polycrystalline structure (Poly).
5. the preparation method of TEM sample as claimed in claim 4, it is characterized in that, described observation and analysis is that U-shaped is cut degree of injury, cutter position, gate oxygen structure, silicon substrate structure, polycrystalline structure, electron beam platinum, ion beam platinum are stopped in front and back, and thickness of sample to be revised and homogeneity one of them or its combination of characterizing.
6. the preparation method of TEM sample as claimed in claim 1 is characterized in that, the thickness of described TEM sample is 90～100nm.
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| CN2013102629085A CN103308365A (en) | 2013-06-27 | 2013-06-27 | Method for preparing triethylenemelamine (TEM) sample |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103913358A (en) * | 2014-04-10 | 2014-07-09 | 武汉新芯集成电路制造有限公司 | Preparation method and failure analysis method for transmission electron microscope (TEM) sample |
| CN104697836A (en) * | 2015-03-30 | 2015-06-10 | 上海华力微电子有限公司 | TEM sample preparation method |
| CN104792583A (en) * | 2014-01-17 | 2015-07-22 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of TEM sample |
| CN105136543A (en) * | 2015-09-27 | 2015-12-09 | 上海华力微电子有限公司 | Preparation method of TEM (Transmission Electron Microscope) sample |
| CN110082567A (en) * | 2019-04-22 | 2019-08-02 | 南京理工大学 | A kind of method of rotary preparation three-dimensional atom probe sample |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110082567A (en) * | 2019-04-22 | 2019-08-02 | 南京理工大学 | A kind of method of rotary preparation three-dimensional atom probe sample |
| CN110082567B (en) * | 2019-04-22 | 2022-03-18 | 南京理工大学 | A method for preparing three-dimensional atom probe samples in a rotary manner |
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Application publication date: 20130918 |