CN103278518A - Detection method for chlorinity in oxide layer - Google Patents
Detection method for chlorinity in oxide layer Download PDFInfo
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- CN103278518A CN103278518A CN201310153806XA CN201310153806A CN103278518A CN 103278518 A CN103278518 A CN 103278518A CN 201310153806X A CN201310153806X A CN 201310153806XA CN 201310153806 A CN201310153806 A CN 201310153806A CN 103278518 A CN103278518 A CN 103278518A
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- oxide layer
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Abstract
A detection method for chlorinity in an oxide layer is provided by the invention, and comprises the following steps: providing a sample comprising the oxide layer, placing the sample in a total reflection X-ray fluorescence spectrometer, determining test points on the oxide layer, and detecting the chlorinity of the test points through the total reflection X-ray fluorescence spectrometer. In the detection method for the chlorinity in the oxide layer, the chlorinity in the oxide layer is detected by the total reflection X-ray fluorescence spectrometer (TXRF), and therefore the detection time is short and the detection cost is low.
Description
Technical field
The present invention relates to technical field of manufacturing semiconductors, particularly the detection method of the chlorinity in a kind of oxide layer.
Background technology
As everyone knows; oxide layer by thermal oxidation technology formation; can be used for protective seam, dielectric layer and the restraining barrier etc. of semiconductor devices according to different needs, it is very extensive that thermal oxidation technology is used in semiconductor devices, can be described as the foundation stone that semiconductor devices is made.So-called thermal oxide is that silicon (Si) is placed oxygenous (O
2) environment in heat, the reaction of oxygen molecule and silicon atom generates silicon dioxide (SiO
2).The temperature of reaction of thermal oxidation technology is very high, and generally more than 1000 ℃, thermal oxidation technology can form the oxide layer of even compact, but the process time is very long.
Except thermal oxidation technology, oxide layer can also adopt low-pressure chemical vapor deposition (LPCVD) mode to form, and namely forms silicon dioxide (SiO by chemical reaction in the substrate surface deposition
2) film.The raw material that adopts in low-pressure chemical vapor deposition (LPCVD) mode has SiH
4, TEOS or DCS, be divided into high-temperature thermal oxidation and low thermal oxidation according to raw materials used difference, wherein, what with DCS be that raw material reacts is high-temperature thermal oxidation reaction (HTO), namely adopts oxidation reactant DCS (SiH under the high-temperature low-pressure condition
2Cl
2) and nitrous oxide (N
2O) reaction generates silicon dioxide (SiO
2).The temperature of reaction of high-temperature thermal oxidation reaction (HTO) is below 1000 ℃, and its reaction equation is:
SiH
2Cl
2(gas)+2N
2O(gas)→SiO
2(solid)+2N
2(gas)+2HCl(gas)。
Quality and the step covering power of the oxide layer that high-temperature thermal oxidation reaction (HTO) deposition forms are all fine, and still, there is the chlorine pollution problem in high-temperature thermal oxidation reaction (HTO).Because high-temperature thermal oxidation reaction (HTO) is raw material with DCS, DCS is dichlorosilane, the silicon dioxide (SiO of formation
2) generally all contain chlorine (Cl) in the film.The too high meeting of chlorinity causes a lot of defectives, influences the performance of semiconductor devices.For example, in the too much zone of chlorinity, oxidation rate is too fast; Chlorine and pasc reaction produce unsaturated link, make the fixed charge density of oxide film increase; Oxidation induced fault phenomenon can occur, cause oxide film inhomogeneous; Also can produce oxide pinhole, cause leakage problem; And the oxide layer breakdown phenomenon etc.So high-temperature thermal oxidation reaction (HTO) forms after the oxide layer, need in time to detect the chlorinity in the oxide layer, prevent that defective products from flowing into subsequent processing.In manufacture process, will take a sample test the chlorinity in the once oxidation layer general every day.
At present, generally adopt flight time formula ion microprobe (TOF-SIMS) to come chlorine detection content.The resolution of ion microprobe (TOF-SIMS) is high, is mainly used in semiconductor and film analysis.Its principle of work is, utilize the primary ions bundle that focuses on to bombard ionization at sample and go out secondary ion, the asynchronism(-nization) of detector because the secondary ion of different quality flies, secondary ion has been realized the mass spectrum separation by mass-to-charge ratio, and the secondary ion that Collection and analysis separates through mass spectrum just can be learnt the element composition of sample surfaces and body and distribute.Flight time formula ion microprobe (TOF-SIMS) not only can the sampling surface the multielement analysis data, but also the secondary ion image that can provide surperficial a certain element to distribute.
But flight time formula ion microprobe (TOF-SIMS) is very expensive, and general enterprise all can't be equipped with.In the time of need carrying out the chlorinity detection to oxide layer, all be to deliver to special testing agency to detect, the cycle of censorship is long, generally needs week age at least.At present, the chlorinity in the oxide layer is long detection time, and testing cost is also very high.
Summary of the invention
The object of the present invention is to provide the detection method of the chlorinity in a kind of oxide layer, to solve chlorinity long, the high problem of detection cost detection time in the existing oxide layer.
For solving the problems of the technologies described above, the invention provides the detection method of the chlorinity in a kind of oxide layer, the detection method of the chlorinity in the described oxide layer may further comprise the steps:
One sample is provided, and described sample comprises oxide layer;
Described sample is placed full-reflection X fluorescent x ray spectroscopy x instrument;
Determine the test point on the described oxide layer;
Detect the chlorinity of described test point by full-reflection X fluorescent x ray spectroscopy x instrument.
Preferably, in the detection method of the chlorinity in described oxide layer, the quantity of described test point is 3, and the position of 3 test points has nothing in common with each other.
Preferably, in the detection method of the chlorinity in described oxide layer, the test duration of single test point is 20 to 30 minutes.
Preferably, in the detection method of the chlorinity in described oxide layer, described oxide layer is to form by the reaction of the high-temperature oxydation in the low-pressure chemical vapor deposition process.
Preferably, in the detection method of the chlorinity in described oxide layer, the oxidation reactant that described high-temperature oxydation reaction is adopted is DCS.
Preferably, in the detection method of the chlorinity in described oxide layer, described oxide layer is silica membrane.
In the detection method of the chlorinity in oxide layer provided by the invention, adopt the chlorinity in full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) the detection oxide layer, and full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) is checkout equipment commonly used in the semiconductor manufacturing, the manufacturer that need carry out semiconductor test all can be equipped with this equipment basically, in addition, the analysis speed of full-reflection X fluorescent x ray spectroscopy x instrument is very fast, and single-spot testing only needs 20～30 minutes.This shows that adopt the chlorinity in full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) the detection oxide layer, detection time is short, and it is low to detect cost.
Description of drawings
Fig. 1 is the schematic flow sheet of the detection method of the chlorinity in the oxide layer of the embodiment of the invention;
Fig. 2 is the correlativity statistical graph of the chlorinity testing result of the chlorinity testing result of TXRF and TOF-SIMS.
Embodiment
Be described in further detail below in conjunction with the detection method of the drawings and specific embodiments to the chlorinity in the oxide layer of the present invention's proposition.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 purpose of the aid illustration embodiment of the invention lucidly.
Chlorinity in the oxide layer detects and need not the ultimate analysis image, so can replace flight time formula ion microprobe (TOF-SIMS) equipment to detect with full-reflection X fluorescent x ray spectroscopy x instrument (TXRF).Please refer to Fig. 1, it is the schematic flow sheet of the detection method of the chlorinity in the oxide layer of the embodiment of the invention.As shown in Figure 1, the detection method of the chlorinity in the described oxide layer comprises the steps:
S10: a sample is provided, and described sample comprises oxide layer;
S11: described sample is placed full-reflection X fluorescent x ray spectroscopy x instrument;
S12: determine the test point on the described oxide layer;
S13: the chlorinity that detects described test point by full-reflection X fluorescent x ray spectroscopy x instrument.
Concrete, sample is to form oxide layer by the reaction of the high-temperature oxydation in the low-pressure chemical vapor deposition process (LPCVD) (HTO), namely under the high-temperature low-pressure condition is that oxidation reactant carries out oxidation reaction and generates silicon dioxide (SiO with DCS
2) film.Oxide layer to high-temperature oxydation reaction (HTO) formation, carry out chlorinity when detecting, at first, sample is put into full-reflection X fluorescent x ray spectroscopy x instrument (TXRF), afterwards, the test point of choosing three diverse locations in oxide layer is carried out chlorinity and is detected.The test duration of a test point probably needs 20～30 minutes, then two other test point is tested after a test point is finished again, and test process is identical, the general detection that just can finish chlorinity in 1 hour.As seen, testing process is very easy, and detection time is very short.
The principle of work of X-ray fluorescence spectra analysis is the atom of x-ray bombardment on excited sample on the sample, to make it to radiate the X ray with energy feature.The energy of these X ray of Collection and analysis and intensity then can be known kind and the content of various elements in the sample.Characteristic X-ray energy and wavelength that different elements send have nothing in common with each other, therefore by the energy of X ray or the measurement of wavelength are known that namely it is which kind of element sends, and carries out the qualitative analysis of element.Simultaneously, the characteristic X ray strength of a certain element is relevant with the content of this element in sample, therefore measures its intensity and just can carry out the quantitative test of element.
And full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) utilizes the total reflection technology, makes the general X-ray fluorescence spectra analyser (XRF) of spuious background ratio of fluorescent reduce about four magnitudes, has improved the sensitivity and the degree of accuracy that detect especially greatly.
Use full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) to carry out the detection of chlorinity, very easy to be quick.High-temperature thermal oxidation reaction (HTO) forms after the oxide layer, can detect the chlorinity in the oxide layer immediately, and detection time is shorter, can prevent effectively that the too high product of chlorinity from flowing into subsequent processing.
And full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) is checkout equipment commonly used during semiconductor is made, and the manufacturer that generally need carry out semiconductor test all can be equipped with this equipment basically.Thus, utilize the chlorinity in full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) the detection oxide layer, we can say to need not to increase cost substantially.
Please continue with reference to figure 2, it is the correlativity statistical graph of the chlorinity testing result of the chlorinity testing result of TXRF and TOF-SIMS.As shown in Figure 2, the correlativity between them coefficient is 0.9389.As seen, full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) chlorine detection content is consistent with the result of flight time formula ion microprobe (TOF-SIMS) chlorine detection content.Yet, adopt full-reflection X fluorescent x ray spectroscopy x instrument (TXRF) the relative ion microprobe of chlorine detection content (TOF-SIMS) chlorine detection content easier fast, and it is lower to detect cost.
To sum up, in the detection method of the chlorinity in the oxide layer that the embodiment of the invention provides, semiconductor devices can adopt full-reflection X fluorescent x ray spectroscopy x instrument to carry out the detection of chlorinity after forming oxide layer immediately, need not to deliver to special testing agency detects, detect easier fast, it is cheaper to detect cost.
Foregoing description only is the description to preferred embodiment of the present invention, is not any restriction to the scope of the invention, and any change, modification that the those of ordinary skill in field of the present invention is done according to above-mentioned disclosure all belong to the protection domain of claims.
Claims (6)
1. the detection method of the chlorinity in the oxide layer is characterized in that, comprising:
One sample is provided, and described sample comprises oxide layer;
Described sample is placed full-reflection X fluorescent x ray spectroscopy x instrument;
Determine the test point on the described oxide layer;
Detect the chlorinity of described test point by full-reflection X fluorescent x ray spectroscopy x instrument.
2. the detection method of the chlorinity in the oxide layer as claimed in claim 1 is characterized in that, the quantity of described test point is 3, and the position of 3 test points has nothing in common with each other.
3. the detection method of the chlorinity in the oxide layer as claimed in claim 2 is characterized in that, the test duration of single test point is 20 to 30 minutes.
4. the detection method of the chlorinity in the oxide layer as claimed in claim 1 is characterized in that, described oxide layer is to form by the reaction of the high-temperature oxydation in the low-pressure chemical vapor deposition process.
5. the detection method of the chlorinity in the oxide layer as claimed in claim 4 is characterized in that, the oxidation reactant that described high-temperature oxydation reaction is adopted is DCS.
6. the detection method of the chlorinity in the oxide layer as claimed in claim 1 is characterized in that, described oxide layer is silica membrane.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104390993A (en) * | 2014-11-18 | 2015-03-04 | 天津中环领先材料技术有限公司 | Method for detecting trace elements of 8-inch polished wafer |
| CN106298793A (en) * | 2016-09-30 | 2017-01-04 | 上海华虹宏力半导体制造有限公司 | Autoregistration grid flash memory device and manufacture method thereof |
| CN106770408A (en) * | 2017-01-05 | 2017-05-31 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN109030528A (en) * | 2018-09-26 | 2018-12-18 | 云南驰宏锌锗股份有限公司 | A kind of method that X-ray fluorescence spectra analyzes fluorine chlorine in smelting smoke dust |
| CN109283298A (en) * | 2018-11-13 | 2019-01-29 | 中国科学院微电子研究所 | SiC-SiO in SiC oxidation2The measuring method and its application of interface carbon residual concentration |
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| CN103063692A (en) * | 2012-12-31 | 2013-04-24 | 上海申和热磁电子有限公司 | Roasting method and detection method for heavy metal in silicon wafer |
| US8481142B1 (en) * | 2005-08-30 | 2013-07-09 | National Semiconductor Corporation | System and method for monitoring chloride content and concentration induced by a metal etch process |
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| DE10138428B4 (en) * | 2001-08-06 | 2004-07-22 | Ech Elektrochemie Halle Gmbh | Method for the summary determination of organochlorine, organobromine, organoiodine and / or organosulfur compounds |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104390993A (en) * | 2014-11-18 | 2015-03-04 | 天津中环领先材料技术有限公司 | Method for detecting trace elements of 8-inch polished wafer |
| CN106298793A (en) * | 2016-09-30 | 2017-01-04 | 上海华虹宏力半导体制造有限公司 | Autoregistration grid flash memory device and manufacture method thereof |
| CN106298793B (en) * | 2016-09-30 | 2019-02-05 | 上海华虹宏力半导体制造有限公司 | Autoregistration grid flash memory device and its manufacturing method |
| CN106770408A (en) * | 2017-01-05 | 2017-05-31 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN106770408B (en) * | 2017-01-05 | 2019-09-27 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN109030528A (en) * | 2018-09-26 | 2018-12-18 | 云南驰宏锌锗股份有限公司 | A kind of method that X-ray fluorescence spectra analyzes fluorine chlorine in smelting smoke dust |
| CN109283298A (en) * | 2018-11-13 | 2019-01-29 | 中国科学院微电子研究所 | SiC-SiO in SiC oxidation2The measuring method and its application of interface carbon residual concentration |
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Application publication date: 20130904 |