CN104155390A - Preparation method and detection method of semiconductor element trace element detection sample - Google Patents
Preparation method and detection method of semiconductor element trace element detection sample Download PDFInfo
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- CN104155390A CN104155390A CN201410359474.5A CN201410359474A CN104155390A CN 104155390 A CN104155390 A CN 104155390A CN 201410359474 A CN201410359474 A CN 201410359474A CN 104155390 A CN104155390 A CN 104155390A
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Abstract
The invention discloses a preparation method and a detection method of a semiconductor element trace element detection sample. The preparation method comprises the following steps: cast-molding a detection sample; cutting the cast-molded detection sample to enable a cut surface to be close to a to-be-analyzed area; polishing the cut surface to enable the to-be-analyzed area to be exposed; and sending the detection sample into a TOF-SIMS high-vacuum chamber, and cleaning the cut surface of the detection sample by utilizing an ion gun so as to remove impurities which are adsorbed onto the cut surface in the cutting and polishing process. No novel pollutant is introduced in the preparation process of the detection sample, and an interface of the detection sample can really reflect the internal situation of the sample by virtue of a series of polishing and cleaning steps. According to the detection method, the prepared detection sample is subject to the surface analysis by virtue of TOF-SIMS, and real element distribution information of a deep cut surface of the sample can be shown, so that deep trace elements can be effectively detected.
Description
Technical field
The present invention relates to technical field of semiconductors, particularly relate to a kind of preparation method and detection method of semiconductor element trace element detection sample.
Background technology
In semiconductor is manufactured, because step is various, be easy to micro-polluter and sneak in semiconductor element.These pollutants can cause the electronic component cannot be by conformity testing, but and prior art means are difficult to such sample to carry out the analysis of effective system.
Conventional analysis means for example the accuracy of detection of SEM, XPS and TEM all in 1% left and right.Polluter lower than 1% is difficult to detected.
Time of flight secondary ion massspectrometry (Time of Flight Secondary Ion Mass Spectrometry, TOF-SIMS) be one of surface analysis technique that current precision is the highest, its advantage is to analyze whole elements, unlike SEM, XPS and TEM, to detecting the units such as H, have limitation.And the accuracy of detection of TOF-SIMS can reach the rank of ppm (1,000,000/), for analyzing trace element, there is very large advantage.
TOF-SIMS also can carry out depth analysis, but analysis speed is slower, especially for the degree of depth on distance surface tens even the analysis of hundreds of micron be unpractical.
Summary of the invention
The object of the invention is to, a kind of preparation method and detection method of semiconductor element trace element detection sample is provided, deep layer trace element is carried out to efficient high-precision analysis.
The preparation method of semiconductor element trace element detection sample provided by the invention, the method comprises:
To detecting sample, carry out mold processing;
The detection sample that cutting mold completes, makes cut surface approach region to be analyzed;
Described cut surface is carried out to polishing, come out in region to be analyzed;
Described detection sample is sent in TOF-SIMS high vacuum chamber, utilized ion gun to clear up to remove to described detection sample cut surface the impurity that is adsorbed on tangent plane in cutting and polishing process.
Optionally, for the preparation method of described semiconductor element trace element detection sample, describedly to detecting sample, carry out mold and be treated to and adopt epoxide-resin glue to carry out mold to detecting sample, sample is all wrapped in epoxide-resin glue.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described epoxide-resin glue is that the component proportioning that hardening agent and epoxy resin are 2.5:16.2 according to mass ratio forms.
Optionally, for the preparation method of described semiconductor element trace element detection sample, the time that described mold is processed is more than 24 hours.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described polishing is for to be polished to cut surface the smooth degree of test request with sand paper, diamond polishing cloth and polishing fluid.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described polishing is for successively peeling off to reach the smooth degree of test request to sample cut surface with Ion Miller.
Optionally, for the preparation method of described semiconductor element trace element detection sample, as need detect metallic element, use O
2+ion gun is cleared up tangent plane; As need detect nonmetalloid, use Cs
+ion gun is cleared up tangent plane.
Optionally, for the preparation method of described semiconductor element trace element detection sample, the cleaning degree of depth is 1nm～1000nm.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described detection sample is multi-level semiconductor structure, and layer depth is more than 10 μ m.
The present invention also provides a kind of detection method of semiconductor element trace element detection sample, comprise: in the preparation method who utilizes described semiconductor element trace element detection sample, make after test sample, with TOF-SIMS, sample is carried out to secondary ion analysis, draw ionic spectrum and ion distribution figure.
Optionally, for the detection method of described semiconductor element trace element detection sample, described secondary ion analysis comprises mass spectrophotometry and imaging analysis.
Optionally, for the detection method of described semiconductor element trace element detection sample, the concentration of element of required detection is lower than 1%.
Compared with prior art, in the preparation method and detection method of semiconductor element trace element detection sample provided by the invention, by carrying out mold to detecting sample, cutting, polishing, ion cleaning and last surface analysis, detect the trace element detecting in sample deep layer.Detect in sample preparation process and do not introduce new pollutant, after a series of polishing and cleanup step, detect the situation that example interface can truly reflect sample interior, and then the surface analysis of TOF-SIMS can provide the true element distributed intelligence of sample deep layer tangent plane, thereby realized the effective detection to deep layer trace element.
Accompanying drawing explanation
Fig. 1 is the preparation method's of embodiment of the present invention semiconductor element trace element detection sample process flow diagram.
Embodiment
Below in conjunction with schematic diagram, preparation method and the detection method of semiconductor element trace element detection sample of the present invention are described in more detail, the preferred embodiments of the present invention have wherein been represented, should be appreciated that those skilled in the art can revise the present invention described here, and still realize advantageous effects of the present invention.Therefore, following description is appreciated that extensively knowing for those skilled in the art, and not as limitation of the present invention.
For clear, whole features of practical embodiments are not described.They in the following description, are not described in detail known function and structure, because can make the present invention chaotic due to unnecessary details.Will be understood that in the exploitation of any practical embodiments, must make a large amount of implementation details to realize developer's specific objective, for example, according to the restriction of relevant system or relevant business, by an embodiment, change into another embodiment.In addition, will be understood that this development may be complicated and time-consuming, but be only routine work to those skilled in the art.
In the following passage, with reference to accompanying drawing, with way of example, the present invention is more specifically described.According to the following describes and claims, advantages and features of the invention will be clearer.It should be noted that, accompanying drawing all adopts very the form of simplifying and all uses non-ratio accurately, only in order to convenient, the object of the aid illustration embodiment of the present invention lucidly.
Core concept of the present invention is: by mold, and cutting, polishing, ion cleaning obtains and detects sample, guarantee not introduce new pollutant in sample preparation process, after a series of polishing and cleanup step, example interface can truly reflect the situation of sample interior.Utilize afterwards TOF-SIMS to detect the trace element in sample deep layer, can provide the true element distributed intelligence of sample deep layer tangent plane.
Based on this thought, the invention provides the preparation method of following semiconductor element trace element detection sample, please refer to Fig. 1, this method comprises:
Step S101: carry out mold processing to detecting sample.Preferably, the present invention is mainly applicable to multi-level semiconductor structure, and layer depth, more than 10 μ m, is the semiconductor samples of 10 μ m, 50 μ m, 100 μ m, 200 μ m etc. such as layer depth, is difficult to carry out conventional TOF-SIMS depth analysis.And need the concentration of element detecting lower than 1%, be unfavorable for carrying out EDX or XPS analysis.In addition, need to guarantee to detect sample and do not damage, there is no crack, to avoid introducing foreign matter.Certainly, for other semiconductor structures, method of the present invention is applicable too.
Concrete, the mold carrying out in this step is treated to and adopts epoxide-resin glue (epoxy) to carry out mold to detecting sample, and sample is all wrapped in epoxide-resin glue.In order to obtain preferably effect, the time that described mold is processed is more than 24 hours.
In a preferred embodiment, described epoxide-resin glue (epoxy) is that the component proportioning that hardening agent (hardner) and epoxy resin (epoxy_resin) are 2.5:16.2 according to mass ratio forms.The ratio of described hardening agent and epoxy resin is not strictly limited to this, can carry out suitable adjustment according to actual needs.
Then, carry out step S102: the detection sample that cutting mold completes, makes cut surface approach region to be analyzed.Cut surface is to the distance in region to be analyzed and be not specifically limited, conventionally can be in tens nanometers between hundreds of nanometer, and such as 50nm, 100nm etc.
Then, carry out step S103: described cut surface is carried out to polishing, come out in region to be analyzed.Preferably, described polishing is for to be polished to cut surface the smooth degree of test request with sand paper, diamond polishing cloth and polishing fluid.
In addition, in another preferred embodiment, described polishing also can be for successively peeling off to reach the smooth degree of test request to sample cut surface with Ion Miller.For example can use Ar
+ion gun carries out polishing to detecting sample.
The polishing of this step take accomplish tangent plane accomplish smooth as good, thereby be convenient to follow-up detection.
Then, carry out step S104: described detection sample is sent in TOF-SIMS high vacuum chamber, utilized ion gun to clear up to remove to described detection sample cut surface the impurity that is adsorbed on tangent plane in cutting and polishing process.This scale removal process is taked different cleaning methods according to the difference of the element of needs detection, and concrete, as need detect metallic element, such as sodium, potassium etc., uses O
2+ion gun is cleared up tangent plane; As need detect nonmetalloid, such as fluorine, oxygen etc., uses Cs
+ion gun is cleared up tangent plane.The degree of depth of described cleaning is 1nm～1000nm.The object of this step is to clean out detecting the impurity that may introduce in the preparation process of sample.
Through above-mentioned steps, can obtain not contaminated detection sample.
Accordingly, the invention provides the detection method to above-mentioned detection sample, preparation method at the semiconductor element trace element detection sample through described makes after test sample, with TOF-SIMS, sample is carried out to secondary ion analysis, preferably, the secondary ion analysis adopting comprises mass spectrophotometry and imaging analysis, to draw ionic spectrum and ion distribution figure.
In the preparation method and detection method of semiconductor element trace element detection sample provided by the invention, by carrying out mold to detecting sample, cutting, polishing, ion cleaning and last surface analysis, detect the trace element detecting in sample deep layer.Detect in sample preparation process and do not introduce new pollutant, after a series of polishing and cleanup step, example interface can truly reflect the situation of sample interior, and then the surface analysis of TOF-SIMS can provide the true element distributed intelligence of sample deep layer tangent plane, thereby realized the effective detection to deep layer trace element.
Obviously, those skilled in the art can carry out various changes and modification and not depart from the spirit and scope of the present invention the present invention.Like this, if within of the present invention these are revised and modification belongs to the scope of the claims in the present invention and equivalent technologies thereof, the present invention is also intended to comprise these changes and modification interior.
Claims (12)
1. a preparation method for semiconductor element trace element detection sample, the method comprises:
To detecting sample, carry out mold processing;
The detection sample that cutting mold completes, makes cut surface approach region to be analyzed;
Described cut surface is carried out to polishing, come out in region to be analyzed;
Described detection sample is sent in TOF-SIMS high vacuum chamber, utilized ion gun to clear up to remove to described detection sample cut surface the impurity that is adsorbed on tangent plane in cutting and polishing process.
2. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, is characterized in that, describedly to detecting sample, carries out mold and is treated to and adopts epoxide-resin glue to carry out mold to detecting sample, and sample is all wrapped in epoxide-resin glue.
3. the preparation method of semiconductor element trace element detection sample as claimed in claim 2, is characterized in that, described epoxide-resin glue is that the component proportioning that hardening agent and epoxy resin are 2.5:16.2 according to mass ratio forms.
4. the preparation method of semiconductor element trace element detection sample as claimed in claim 3, is characterized in that, the time that described mold is processed is more than 24 hours.
5. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, is characterized in that, described polishing is for to be polished to cut surface the smooth degree of test request with sand paper, diamond polishing cloth and polishing fluid.
6. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, is characterized in that, described polishing is for successively peeling off to reach the smooth degree of test request to sample cut surface with Ion Miller.
7. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, is characterized in that, as need detect metallic element, uses O
2+ion gun is cleared up tangent plane; As need detect nonmetalloid, use Cs
+ion gun is cleared up tangent plane.
8. the preparation method of semiconductor element trace element detection sample as claimed in claim 7, is characterized in that, the cleaning degree of depth is 1nm～1000nm.
9. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, is characterized in that, described detection sample is multi-level semiconductor structure, and layer depth is more than 10 μ m.
10. the detection method of a semiconductor element trace element detection sample, comprise: the preparation method who utilizes the semiconductor element trace element detection sample as described in any one in claim 1～9, after making test sample, with TOF-SIMS, sample is carried out to secondary ion analysis, draw ionic spectrum and ion distribution figure.
The detection method of 11. semiconductor element trace element detection samples as claimed in claim 10, is characterized in that, described secondary ion analysis comprises mass spectrophotometry and imaging analysis.
The detection method of 12. semiconductor element trace element detection samples as claimed in claim 10, is characterized in that, the concentration of element of required detection is lower than 1%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106770185A (en) * | 2016-12-28 | 2017-05-31 | 湖北省地质实验测试中心 | A kind of elemental detection system and detection method based on ccd sensor |
| CN107449648A (en) * | 2017-06-30 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of preparation method of the sample target of ore mineral suitable for ion microprobe analysis |
| CN109001240A (en) * | 2018-08-17 | 2018-12-14 | 胜科纳米（苏州）有限公司 | The method for preparing non-conductive material sample |
| CN113588372A (en) * | 2021-08-13 | 2021-11-02 | 胜科纳米(苏州)股份有限公司 | Sample preparation method and detection method for measuring element diffusion of VCSEL device multilayer film |
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| US5920068A (en) * | 1998-03-05 | 1999-07-06 | Micron Technology, Inc. | Analysis of semiconductor surfaces by secondary ion mass spectrometry |
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| A. BESMEHN等: "Surface characterisation and interface studies of high-k materials by XPS and TOF-SIMS", 《APPLIED SURFACE SCIENCE》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770185A (en) * | 2016-12-28 | 2017-05-31 | 湖北省地质实验测试中心 | A kind of elemental detection system and detection method based on ccd sensor |
| CN107449648A (en) * | 2017-06-30 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of preparation method of the sample target of ore mineral suitable for ion microprobe analysis |
| CN107449648B (en) * | 2017-06-30 | 2019-09-27 | 中国科学院广州地球化学研究所 | A kind of preparation method of the sample target of the ore mineral suitable for ion microprobe analysis |
| CN109001240A (en) * | 2018-08-17 | 2018-12-14 | 胜科纳米（苏州）有限公司 | The method for preparing non-conductive material sample |
| CN113588372A (en) * | 2021-08-13 | 2021-11-02 | 胜科纳米(苏州)股份有限公司 | Sample preparation method and detection method for measuring element diffusion of VCSEL device multilayer film |
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