CN105486553A - Preparation method of transmission electron microscope test piece - Google Patents
Preparation method of transmission electron microscope test piece Download PDFInfo
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- CN105486553A CN105486553A CN201410477540.9A CN201410477540A CN105486553A CN 105486553 A CN105486553 A CN 105486553A CN 201410477540 A CN201410477540 A CN 201410477540A CN 105486553 A CN105486553 A CN 105486553A
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- electron microscope
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- type electron
- penetration type
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 230000005540 biological transmission Effects 0.000 title claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 24
- 230000035515 penetration Effects 0.000 claims description 98
- 238000000034 method Methods 0.000 claims description 58
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 238000005520 cutting process Methods 0.000 claims description 20
- 238000010884 ion-beam technique Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 239000013043 chemical agent Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 240000001439 Opuntia Species 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of a transmission electron microscope test piece, which comprises the following steps. The first thinning treatment is carried out on the observed object, and a transmission electron microscope test piece with the thickness resistant to the chemical treatment is formed in the preset observation area of the observed object. The chemical treatment was carried out at room temperature on the piece of the transmission electron microscope. And performing a second thinning treatment on the chemically treated transmission electron microscope test piece to make the transmission electron microscope test piece have a thickness for being observed by a transmission electron microscope. The transmission electron microscope test piece was taken out from the observation object.
Description
Technical field
The present invention relates to a kind of preparation method of test piece, and particularly relate to the preparation method of a kind of transmission electron microscope (transmissionelectronmicroscope, TEM) test piece.
Background technology
In semiconductor fabrication process, when manufacture craft material and defective material have the identical crystalline texture be made up of different element, be sometimes difficult to distinguish its interface in transmission electron microscope is observed, and the location of defect cannot be judged significantly.
Therefore, develop in a kind of process preparing test piece of penetration type electron microscope at present, add chemically treated technology, the thickness of test piece that different materials can be made to present after etching is different and be easy to tell in transmission electron microscope the location of defect.
The preparation method of common test piece of penetration type electron microscope mainly can classify as following two kinds of modes.Use the lapping mode of abrasive cloth to be test piece be directly ground to supply transmission electron microscope to carry out the thickness observed, then chemical treatment is carried out to this test piece.But, because the thickness of test piece after grinding is very thin, so rate of etch must be controlled by controlling chemically treated temperature, damage to avoid test piece.In addition, the lapping mode of abrasive cloth is used cannot to provide the defect analysis of fixed point microcell.
The preparation method of another kind of electronic microscope test block utilizes after focused ion beam prepares the test piece of penetration type electron microscope of fixed point micro-zone analysis, then carries out chemical treatment to this test piece.Similarly, because the thickness of the observation area of the test piece after line focus Ion Beam Treatment is very thin, so rate of etch must be controlled by controlling chemically treated temperature, damage to avoid test piece.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of test piece of penetration type electron microscope, it at room temperature can carry out chemical treatment to test piece of penetration type electron microscope, and can not cause damage to test piece of penetration type electron microscope.
For reaching above-mentioned purpose, the present invention proposes a kind of preparation method of test piece of penetration type electron microscope, comprises the following steps.First thinning process is carried out to the object of observation, and in the predetermined observation area of the object of observation, forms the test piece of penetration type electron microscope with the thickness of chemically-resistant process.At room temperature chemical treatment is carried out to test piece of penetration type electron microscope.Carry out the second thinning process to through chemically treated test piece of penetration type electron microscope, test piece of penetration type electron microscope is had and supplies transmission electron microscope to carry out the thickness observed.Test piece of penetration type electron microscope is taken out from the object of observation.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, the first thinning processing example uses focused ion beam to carry out in this way.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, the first thinning process can be the thinning process of single track manufacture craft or multiple tracks manufacture craft thinning process.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, multiple tracks manufacture craft thinning process comprises first carries out thick thinning process to the object of observation, then carries out thin thinning process to the object of observation.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, chemical treatment is such as doped solution dip treating (dopant-solutiondip) or oxide etch solution dip treating (oxide-etchingsolutiondip).
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, the second thinning process comprises use focused ion beam and carries out.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, after carrying out chemical treatment, also comprise and soaked cleaning treatment is carried out to test piece of penetration type electron microscope.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, after carrying out soaked cleaning treatment, also comprise and heating, drying process is carried out to test piece of penetration type electron microscope.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, the method for taking out test piece of penetration type electron microscope from the object of observation is such as carry out single track cutting manufacture craft or multiple tracks cutting manufacture craft.
Described in one embodiment of the invention, in the preparation method of above-mentioned test piece of penetration type electron microscope, multiple tracks cutting manufacture craft comprises the following steps.After carrying out chemical treatment, carry out U-shaped cutting to this predetermined observation of this object of observation, now test piece of penetration type electron microscope not yet cuts from the object of observation, and forms connecting portion between test piece of penetration type electron microscope and the object of observation.After carrying out the second thinning process, cut off connecting portion, and test piece of penetration type electron microscope is taken out from the object of observation.
Based on above-mentioned, in the preparation method of test piece of penetration type electron microscope proposed by the invention, because the test piece of penetration type electron microscope after carrying out the first thinning process to the object of observation has the thickness of chemically-resistant process, so have preferably test piece intensity.Therefore, even if at room temperature carry out chemical treatment to test piece of penetration type electron microscope, also damage can not be caused to test piece of penetration type electron microscope.In addition, the preparation method due to test piece of penetration type electron microscope proposed by the invention forms test piece of penetration type electron microscope in predetermined observation area, therefore can be used for the defect analysis of fixed point microcell.
For above-mentioned feature and advantage of the present invention can be become apparent, special embodiment below, and the accompanying drawing appended by coordinating is described in detail below.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of the test piece of penetration type electron microscope of one embodiment of the invention;
Fig. 2 A to Fig. 2 C is respectively the top view of the object of observation after the thinning process of step S102, step S104 and the step S150 carried out in Fig. 1 and test piece of penetration type electron microscope;
Schematic diagram when Fig. 3 is the chemical treatment of the step S110 carried out in Fig. 1, and Fig. 3 draws along the I-I ' profile line in Fig. 2 B;
Fig. 4 A and Fig. 4 B is respectively the schematic diagram during cutting process carrying out step S140 in Fig. 1 and step S160, and Fig. 4 A and Fig. 4 B draws along the II-II ' profile line in Fig. 2 B and Fig. 2 C.
Symbol description
100: the object of observation
102: predetermined observation area
104: test piece of penetration type electron microscope
106: groove
108: connecting portion
200: test tube
202: chemical agent
S100, S102, S104, S110, S120, S130, S140, S150, S160: step numbers
T1, T2, T3: thickness
Embodiment
Fig. 1 illustrate the preparation flow figure of the test piece of penetration type electron microscope into one embodiment of the invention.Fig. 2 A to Fig. 2 C is respectively the top view of the object of observation after the thinning process of step S102, step S104 and the step S150 carried out in Fig. 1 and test piece of penetration type electron microscope.Schematic diagram when Fig. 3 is the chemical treatment of the step S110 carried out in Fig. 1, and Fig. 3 draws along the I-I ' profile line in Fig. 2 B.Fig. 4 A and Fig. 4 B is respectively the schematic diagram during cutting process carrying out step S140 in Fig. 1 and step S160, and Fig. 4 A and Fig. 4 B draws along the II-II ' profile line in Fig. 2 B and Fig. 2 C.
Referring to Fig. 1, Fig. 2 A and Fig. 2 B, first, carry out step S100, the first thinning process is carried out to the object of observation 100, and in the predetermined observation area 102 of the object of observation 100, form the test piece of penetration type electron microscope 104 with the thickness T2 of chemically-resistant process.Meanwhile, groove 106 can be formed in test piece of penetration type electron microscope 104 both sides.The object of observation 100 is such as semi-conductor chip.Predetermined observation area 102 is such as metal oxide semiconductor transistor (metaloxidesemiconductor (MOS) transistor) element region.First thinning processing example uses focused ion beam to carry out in this way.The thickness T2 of chemically-resistant process is such as 0.35 micron to 0.5 micron, but the present invention is not as limit.In the present embodiment, the thickness T2 of chemically-resistant process is described for 0.35 micron.
In the step s 100, the first thinning process is treated to example with the thinning of multiple tracks manufacture craft to be described.Multiple tracks manufacture craft thinning process comprises the following steps.First, carry out step S102, thick (coarse) thinning process (please refer to Fig. 2 A) is carried out to the object of observation 100.Thick thinning processing example is carried out with the focused ion beam being greater than 300pA in this way.Now, the thickness T1 of test piece of penetration type electron microscope 104 is such as 0.5 micron to 1.0 microns, but the present invention is not as limit.In the present embodiment, thickness T1 is described for 0.5 micron.
Then, carry out step S104, thin (fine) thinning process (please refer to Fig. 2 B) is carried out to the object of observation 100.Thin thinning process can be pruned in thick thinning process by the part that high-energy focusing ion beam damages.Thin thinning processing example is carried out with the focused ion beam being less than 100pA in this way.Now, although the thickness T2 of test piece of penetration type electron microscope 104 is less than thickness T1, but thickness T2 still keeps the thickness being enough to chemically-resistant process, test piece of penetration type electron microscope 104 can be made can to have enough test piece intensity and to cause damage to prevent chemical treatment.As mentioned above, the thickness T2 of the chemically-resistant process in the present embodiment is described for 0.35 micron.
In this embodiment, although the first thinning process is treated to example with the thinning of multiple tracks manufacture craft to be described, the present invention is not as limit.In other embodiments, the first thinning process also can adopt single track manufacture craft thinning process in predetermined observation area 102, directly form the test piece of penetration type electron microscope 104 with the thickness T2 of chemically-resistant process.
Then, referring to Fig. 1 and Fig. 3, carry out step S110, at room temperature chemical treatment is carried out to test piece of penetration type electron microscope 104.Chemical treatment is such as admixture (doping) solution impregnation process or oxide etch solution dip treating, but the present invention is not as limit.Art has knows that the knowledgeable can according to the element material of wanted observation analysis usually, and the chemical agent needed for selection carries out chemical treatment to test piece of penetration type electron microscope 104.For example, test tube 200 can be used to be added drop-wise in groove 106 by chemical agent 202, chemical agent 202 be contacted with test piece of penetration type electron microscope 104, and carries out chemical treatment.
Next, continue referring to Fig. 1, optionally carry out step S120, soaked cleaning treatment is carried out to test piece of penetration type electron microscope 104, to remove the chemical agent on test piece of penetration type electron microscope 104.
Afterwards, optionally carry out step S130, heating, drying process is carried out to test piece of penetration type electron microscope 104, water stain to remove.
Moreover, referring to Fig. 1 and Fig. 4 A, carry out step S140, U-shaped cutting is carried out to the predetermined observation area 102 of the object of observation 100, now test piece of penetration type electron microscope 104 not yet cuts from the object of observation 100, and forms connecting portion 108 between test piece of penetration type electron microscope 104 and the object of observation 100.U-shaped cutting is such as use focused ion beam to carry out.When adopting focused ion beam to carry out U-shaped cutting, the electric current of focused ion beam is such as 800 ~ 1200pA.
Then, referring to Fig. 1 and Fig. 2 C, carry out step S150, carry out the second thinning process to through chemically treated test piece of penetration type electron microscope 104, test piece of penetration type electron microscope 104 is had and supplies transmission electron microscope to carry out the thickness T3 observed.In addition, the second thinning process also can to remove when carrying out chemical treatment simultaneously the product that remains, with prevent the region that will analyze cover by the product that remains.Second thinning processing example uses focused ion beam to carry out in this way.Second thinning processing example is carried out with the focused ion beam being less than 100pA in this way.The thickness T3 carrying out observing for transmission electron microscope is such as 0.1 micron to 0.2 micron, but the present invention is not as limit.In the present embodiment, the thickness T3 carrying out observing for transmission electron microscope is described for 0.15 micron.
Subsequently, referring to Fig. 1, Fig. 4 A and Fig. 4 B, carry out step S160, from the object of observation 100, take out test piece of penetration type electron microscope 104.The method of taking out test piece of penetration type electron microscope 104 is such as cut off connecting portion 108, and is taken out from the object of observation 100 by test piece of penetration type electron microscope 104.The method cutting off connecting portion 108 is such as use focused ion beam to carry out.When adopting focused ion tractotomy connecting portion 108, the range of current of focused ion beam is such as be less than 100pA.In addition, when adopting focused ion to prepare test piece of penetration type electron microscope 104, outer samples method (exsitulift-outmethod) or inner sampling method (insitulift-outmethod) can be adopted to take out test piece of penetration type electron microscope 104.
This embodiment be adopt multiple tracks cutting manufacture craft take out test piece of penetration type electron microscope 104, therefore by step S150 the second thinning process by the U-shaped cutting produced pollution thing by step S140 from test piece of penetration type electron microscope 104 removing.In addition, owing to first carrying out U-shaped cutting to test piece of penetration type electron microscope 104 in step S140, therefore, when carrying out step S160 and test piece of penetration type electron microscope 104 being taken out from the object of observation 100, can reduce significantly by the quantity of the cutting manufacture craft produced pollution thing of step S160.
In this embodiment, although be adopt multiple tracks to cut manufacture craft to take out test piece of penetration type electron microscope 104 and be described for example, the present invention is not as limit.In other embodiments, single track also can be adopted to cut manufacture craft and to take out test piece of penetration type electron microscope 104.That is, when the quantity of single track cutting manufacture craft produced pollution thing is in permissible scope, the U-shaped cutting of step S140 can not be carried out, and after the second thinning process carrying out step S150, directly in step S160, test piece of penetration type electron microscope 104 is cut from the object of observation 100.
Known based on above-described embodiment, in the preparation method of the test piece of penetration type electron microscope 104 of above-described embodiment, because the test piece of penetration type electron microscope 104 after carrying out the first thinning process to the object of observation 100 has the thickness T2 of chemically-resistant process, so have preferably test piece intensity.Therefore, even if at room temperature carry out chemical treatment to test piece of penetration type electron microscope 104, also damage can not be caused to test piece of penetration type electron microscope 104.In addition, the preparation method due to the test piece of penetration type electron microscope 104 of above-described embodiment forms test piece of penetration type electron microscope 104 in predetermined observation area 102, therefore can be used for the defect analysis of fixed point microcell.
In sum, above-described embodiment at least has features.The preparation method of the test piece of penetration type electron microscope of above-described embodiment at room temperature can carry out chemical treatment to test piece of penetration type electron microscope, and can not cause damage to test piece of penetration type electron microscope.In addition, the preparation method of the test piece of penetration type electron microscope of above-described embodiment can be used for the defect analysis of fixed point microcell.
Although disclose the present invention in conjunction with above embodiment; but itself and be not used to limit the present invention; have in any art and usually know the knowledgeable; without departing from the spirit and scope of the present invention; a little change and retouching can be done, therefore being as the criterion of should defining with the claim of enclosing of protection scope of the present invention.
Claims (10)
1. a preparation method for test piece of penetration type electron microscope, comprising:
One first thinning process is carried out to an object of observation, and in a predetermined observation area of this object of observation, forms a test piece of penetration type electron microscope with the thickness of a chemically-resistant process;
At room temperature a chemical treatment is carried out to this test piece of penetration type electron microscope;
Carry out one second thinning process to through this this test piece of penetration type electron microscope chemically treated, make this test piece of penetration type electron microscope have one and supply transmission electron microscope to carry out the thickness observed; And
This test piece of penetration type electron microscope is taken out from this object of observation.
2. the preparation method of test piece of penetration type electron microscope as claimed in claim 1, wherein this first thinning process comprises and uses focused ion beam to carry out.
3. the preparation method of test piece of penetration type electron microscope as claimed in claim 1, wherein this first thinning process comprises a single track manufacture craft thinning process or a multiple tracks manufacture craft thinning process.
4. the preparation method of test piece of penetration type electron microscope as claimed in claim 3, wherein this multiple tracks manufacture craft thinning process comprises and first carries out thick thinning process to this object of observation, then carries out thin thinning process to this object of observation.
5. the preparation method of test piece of penetration type electron microscope as claimed in claim 1, wherein this chemical treatment comprises doped solution dip treating or oxide etch solution dip treating.
6. the preparation method of test piece of penetration type electron microscope as claimed in claim 1, wherein this second thinning process comprises and uses focused ion beam to carry out.
7. the preparation method of test piece of penetration type electron microscope as claimed in claim 1, wherein after carrying out this chemical treatment, also comprises and carries out a soaked cleaning treatment to this test piece of penetration type electron microscope.
8. the preparation method of test piece of penetration type electron microscope as claimed in claim 7, wherein after carrying out this soaked cleaning treatment, also comprises and carries out a heating, drying process to this test piece of penetration type electron microscope.
9. the preparation method of test piece of penetration type electron microscope as claimed in claim 1, the method for wherein taking out this test piece of penetration type electron microscope from this object of observation comprises carries out a single track cutting manufacture craft or multiple tracks cutting manufacture craft.
10. the preparation method of test piece of penetration type electron microscope as claimed in claim 9, wherein this multiple tracks cutting manufacture craft comprises:
After carrying out this chemical treatment, U-shaped cutting is carried out to this predetermined observation area of this object of observation, now this test piece of penetration type electron microscope not yet cuts from this object of observation, and between this test piece of penetration type electron microscope and this object of observation, form a junction; And
After carrying out this second thinning process, cut off this connecting portion, and this test piece of penetration type electron microscope is taken out from this object of observation.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW103130120 | 2014-09-01 | ||
| TW103130120A TWI506262B (en) | 2014-09-01 | 2014-09-01 | Method for preparing transmission electron microscope sample |
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| CN105486553A true CN105486553A (en) | 2016-04-13 |
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| CN201410477540.9A Pending CN105486553A (en) | 2014-09-01 | 2014-09-18 | Preparation method of transmission electron microscope test piece |
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| CN (1) | CN105486553A (en) |
| TW (1) | TWI506262B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198147A (en) * | 2016-08-19 | 2016-12-07 | 上海华力微电子有限公司 | The method of example of transmission electron microscope knot dyeing |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI784569B (en) * | 2021-06-11 | 2022-11-21 | 中國鋼鐵股份有限公司 | Preparation method and detection method of microscope specimen |
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Also Published As
| Publication number | Publication date |
|---|---|
| TWI506262B (en) | 2015-11-01 |
| TW201610409A (en) | 2016-03-16 |
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Application publication date: 20160413 |