CN104155390B - Preparation method and the detection method of semiconductor element trace element detection sample - Google Patents
Preparation method and the detection method of semiconductor element trace element detection sample Download PDFInfo
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- CN104155390B CN104155390B CN201410359474.5A CN201410359474A CN104155390B CN 104155390 B CN104155390 B CN 104155390B CN 201410359474 A CN201410359474 A CN 201410359474A CN 104155390 B CN104155390 B CN 104155390B
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Abstract
The present invention has disclosed a kind of preparation method and detection method of semiconductor element trace element detection sample. This preparation method comprises: carry out mold processing to detecting sample; 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. This has ensured to detect in sample preparation process does not introduce new pollutant, after a series of polishing and cleanup step, detects the situation that example interface can truly reflect sample interior. This detection method is carried out surface analysis by TOF-SIMS to the detection sample making can provide the true element distributed intelligence of sample deep layer tangent plane, thereby has realized the effective detection to deep layer trace element.
Description
Technical field
The present invention relates to technical field of semiconductors, particularly relate to a kind of semiconductor element trace element detection sampleThe preparation method of product and detection method.
Background technology
In semiconductor is manufactured, because step is various, be easy to micro-polluter and sneak into semiconductor elementIn part. These pollutants can cause the electronic component cannot be by conformity testing, but and prior art means are difficultIn the analysis of such sample being carried out to effective system.
The accuracy of detection of conventional analysis means for example SEM, XPS and TEM is all in 1% left and right. Lower than1% polluter is difficult to detected.
Time of flight secondary ion massspectrometry (TimeofFlightSecondaryIonMassSpectrometry,TOF-SIMS) be one of surface analysis technique that current precision is the highest, its advantage is can be to whole unitsElement is analyzed, and have limitation unlike SEM, XPS and TEM to detecting the units such as H. And TOF-SIMSAccuracy of detection can reach the rank of ppm (1,000,000/), have very large for analyzing trace elementAdvantage.
TOF-SIMS also can carry out depth analysis, but analysis speed is slower, especially for the degree of depthOn distance surface tens, even the analysis of hundreds of micron is unpractical.
Summary of the invention
The object of the invention is to, provide a kind of semiconductor element trace element detection sample preparation method andDetection method, carries out efficient high-precision analysis to deep layer trace element.
The preparation method of semiconductor element trace element detection sample provided by the invention, the method comprises:
Carry out mold processing to detecting sample;
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 described detection sampleCut surface clears up to remove 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, described to inspectionTest sample product carry out mold be treated to adopt epoxide-resin glue to detect sample carry out mold, sample is all wrapped upIn epoxide-resin glue.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described epoxyResin glue is that the component proportioning that curing 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, described moldThe time of processing is more than 24 hours.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described polishingBe treated to the smooth degree that with sand paper, diamond polishing cloth and polishing fluid, cut surface is polished to test request.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described polishingBe treated to the smooth degree of with Ion Miller, sample cut surface successively being peeled off to reach test request.
Optionally, for the preparation method of described semiconductor element trace element detection sample, detect as neededMetallic element, uses O2+Ion gun is cleared up tangent plane; As need detect nonmetalloid, use Cs+FromSub-rifle is cleared up tangent plane.
Optionally, for the preparation method of described semiconductor element trace element detection sample, the cleaning degree of depthFor 1nm～1000nm.
Optionally, for the preparation method of described semiconductor element trace element detection sample, described detectionSample 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, comprising: in profitMake and test after sample by the preparation method of described semiconductor element trace element detection sample, useTOF-SIMS carries out secondary ion analysis to sample, draws ionic spectrum and ion distribution figure.
Optionally, for the detection method of described semiconductor element trace element detection sample, described secondaryIon analysis comprises mass spectral analysis and imaging analysis.
Optionally, for the detection method of described semiconductor element trace element detection sample, required detectionConcentration of element lower than 1%.
Compared with prior art, the preparation method of semiconductor element trace element detection sample provided by the inventionAnd in detection method, by carrying out mold to detecting sample, cutting, polishing, ion cleaning and lastSurface analysis, detects the trace element detecting in sample deep layer. Detect in sample preparation process and do not haveIntroduce new pollutant, after a series of polishing and cleanup step, detecting example interface can be trueReflect the situation of sample interior, and then the surface analysis of TOF-SIMS can provide sample deep layer tangent planeTrue element distributed intelligence, thus realize the effective detection to deep layer trace element.
Brief description of the drawings
Fig. 1 is the preparation method's of embodiment of the present invention semiconductor element trace element detection sample flow chart.
Detailed description of the invention
Preparation method below in conjunction with schematic diagram to semiconductor element trace element detection sample of the present invention andDetection method is described in more detail, and has wherein represented the preferred embodiments of the present invention to should be appreciated that abilityField technique personnel 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 to the present inventionRestriction.
For clear, whole features of practical embodiments are not described. In the following description, be not described in detail public affairsThe function and structure of knowing, because they can make the present invention chaotic due to unnecessary details. Will be understood thatIn the exploitation of any practical embodiments, must make a large amount of implementation details to realize developer's specific objective,For example, according to about system or about the restriction of business, change into another embodiment by an embodiment. Separately, will be understood that this development may be complicated and time-consuming outward, but for art technology peopleMember is only routine work.
In the following passage, with way of example, the present invention is more specifically described with reference to accompanying drawing. According to the following describes andClaims, advantages and features of the invention will be clearer. It should be noted that, accompanying drawing all adopts very simpleThe form of changing and all use non-ratio accurately, only in order to convenient, the aid illustration embodiment of the present invention lucidlyObject.
Core concept of the present invention is: by mold, and cutting, polishing, ion cleaning obtains and detects sample,Ensure 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 in sample deep layerTrace element detect, can provide the true element distributed intelligence of sample deep layer tangent plane.
Based on this thought, the invention provides the preparation side of following semiconductor element trace element detection sampleMethod, please refer to Fig. 1, and this method comprises:
Step S101: carry out mold processing to detecting sample. Preferably, the present invention is mainly applicable at many levelsSemiconductor structure, layer depth is more than 10 μ m, and such as layer depth is 10 μ m, 50 μ m, 100 μ m, 200 μ m etc.Semiconductor samples, be difficult to carry out conventional TOF-SIMS depth analysis. And need the element of detection denseDegree, lower than 1%, is unfavorable for carrying out EDX or XPS analysis. In addition, need to ensure 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 inventionBe suitable for too.
Concrete, the mold carrying out in this step is treated to and adopts epoxide-resin glue (epoxy) to detecting sampleCarry out mold, sample is all wrapped in epoxide-resin glue. In order to obtain preferably effect, described moldThe time of processing is more than 24 hours.
In a preferred embodiment, described epoxide-resin glue (epoxy) is curing agent (hardner) and ringThe component proportioning that epoxy resins (epoxy_resin) is 2.5:16.2 according to mass ratio forms. Described curing agent and ringThe ratio of epoxy resins 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 district to be analyzedTerritory. Cut surface is to the distance in region to be analyzed and be not specifically limited, conventionally can be in tens nanometers to hundreds ofBetween nanometer, such as 50nm, 100nm etc.
Then, carry out step S103: described cut surface is carried out to polishing, region to be analyzed is exposedOut. Preferably, described polishing is for throwing cut surface with sand paper, diamond polishing cloth and polishing fluidLight is to the smooth degree of test request.
In addition, in another preferred embodiment, described polishing can be also to sample with Ion MillerCut surface successively peels off to reach the smooth degree of test request. For example can use Ar+Ion gun is to inspectionTest sample product carry out polishing.
The polishing of this step taking 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, utilizedIon gun is cleared up to remove to described detection sample cut surface and in cutting and polishing process, is adsorbed on tangent planeImpurity. This scale removal process is taked different cleaning methods according to the difference of the element of needs detection, concrete,As need detect metallic element, such as sodium, potassium etc., use O2+Ion gun is cleared up tangent plane; Detect as neededNonmetalloid, such as fluorine, oxygen etc., use Cs+Ion gun is cleared up tangent plane. The degree of depth of described cleaningFor 1nm～1000nm. The object of this step is detecting the impurity that may introduce in the preparation process of sample clearReason is clean.
Through above-mentioned steps, can obtain not contaminated detection sample.
Accordingly, the invention provides the detection method to above-mentioned detection sample, at the semiconductor element through describedThe preparation method of part trace element detection sample makes after test sample, sample is carried out to two with TOF-SIMSSecondary ion is analyzed, and preferably, the secondary ion analysis of employing comprises mass spectral analysis and imaging analysis, withGo out ionic spectrum and ion distribution figure.
In the preparation method and detection method of semiconductor element trace element detection sample provided by the invention, logicalCross and carry out mold to detecting sample, cutting, polishing, ion cleaning and last surface analysis, to detectingTrace element in sample deep layer detects. 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, therebyRealize 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 this present inventionBright spirit and scope. Like this, if of the present invention these amendment and modification belong to the claims in the present invention andWithin the scope of its equivalent technologies, the present invention be also intended to comprise these change and modification interior.
Claims (9)
1. a preparation method for semiconductor element trace element detection sample, the method comprises:
Carry out mold processing to detecting sample;
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 described detection sampleCut surface clears up to remove 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, its featureBe, described to detect sample carry out mold be treated to adopt epoxide-resin glue to detect sample carry out mold,Sample is all wrapped in epoxide-resin glue.
3. the preparation method of semiconductor element trace element detection sample as claimed in claim 2, its featureBe, described epoxide-resin glue is the component proportioning shape that curing agent and epoxy resin are 2.5:16.2 according to mass ratioBecome.
4. the preparation method of semiconductor element trace element detection sample as claimed in claim 3, its featureBe, the time of described mold processing is more than 24 hours.
5. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, its featureBe, described polishing is for being polished to test with sand paper, diamond polishing cloth and polishing fluid by cut surfaceThe smooth degree requiring.
6. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, its featureBe, described polishing is wanted for sample cut surface successively being peeled off to reach test with Ion MillerThe smooth degree of asking.
7. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, its featureBe, as need detect metallic element, use O2+Ion gun is cleared up tangent plane; As need detect nonmetal unitElement, uses Cs+Ion gun is cleared up tangent plane.
8. the preparation method of semiconductor element trace element detection sample as claimed in claim 7, its featureBe, the cleaning degree of depth is 1nm～1000nm.
9. the preparation method of semiconductor element trace element detection sample as claimed in claim 1, its featureBe, described detection sample is multi-level semiconductor structure, and layer depth is more than 10 μ m.
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| 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 |
| 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 |
| CN109001240B (en) * | 2018-08-17 | 2021-04-13 | 胜科纳米（苏州）有限公司 | Method for preparing non-conductive material sample |
| CN113588372B (en) * | 2021-08-13 | 2022-09-02 | 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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Address after: Room 507, building 09, Northwest District, Suzhou nano City, No. 99, Jinjihu Avenue, Suzhou Industrial Park, China (Jiangsu) pilot Free Trade Zone, Suzhou, Jiangsu 215000 Patentee after: Shengke nano (Suzhou) Co.,Ltd. Address before: Room 507, building 09, northwest Suzhou nano City, 99 Jinjihu Avenue, Suzhou Industrial Park, Jiangsu Province, 215123 Patentee before: SHENGKE NANO (SUZHOU) Co.,Ltd. |
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