CN103165407B - A kind of for the surface treatment of silicon slice surface sample preparation and the technique of corrosion and device - Google Patents
A kind of for the surface treatment of silicon slice surface sample preparation and the technique of corrosion and device Download PDFInfo
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- CN103165407B CN103165407B CN201110417124.6A CN201110417124A CN103165407B CN 103165407 B CN103165407 B CN 103165407B CN 201110417124 A CN201110417124 A CN 201110417124A CN 103165407 B CN103165407 B CN 103165407B
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Abstract
For the surface treatment of silicon slice surface sample preparation and the technique of corrosion and a device, enter in the corrosion cavity of sealing containing ozone in technique, contact with silicon chip surface, silicon chip surface is oxidized to the oxide-film operation of densification.Device comprises: corrosion cavity (1), housing (2), be provided with silicon wafer stage (4) and logical ozone or nitrogen inlet (1-1) in cavity, by nitrogen as the HF gas access (1-2) of carrier and steam vent (1-4), also comprise the HF container (5) of peripheral hardware, the entrance (1-1) of described logical ozone or nitrogen is connected in series valve V2, flow control valve MFC
1, MFC
1another termination threeway, a termination nitrogen pipeline of threeway, the outlet on another termination ozonizer road of threeway.Advantage of the present invention is: ozone can be utilized silicon chip surface first to be formed fine and close oxide-film, again surface film oxide is effectively corroded, and make silicon chip surface be hydrophobicity, be conducive to next step with the scanning of drop to silicon chip hydrophobic surface and the collection of metal impurities, simple process, apparatus structure is compact, easy to operate, effective.
Description
Technical field
The present invention relates to a kind of etching process of silicon slice surface sample preparation and the improvement of device, be particularly useful for the silicon chip that surface only has natural oxide film.
Background technology
Silicon chip is most popular backing material in integrated circuit, in the processing technology of semiconductor, there is the yield loss rate more than 50% to be caused by the pollution of silicon face, along with the raising day by day of circuit level, unit figure size is day by day microminiaturized, and pollutant is also further outstanding on the impact of device.Metal contamination can destroy integrality, increase leakage current density, the minimizing minority carrier life time of thin oxide layer, affects the stability of MOS device.When metal contamination is serious, also can form vaporific defect (Haze). therefore, we need to carry out metal contamination test to silicon chip, and object confirms on silicon chip, whether in allowed limits metal contamination, in the procedure entered subsequently to avoid defective item.
Before use ICP-MS (inductivity coupled plasma mass spectrometry analysis), TXRF (x-ray fluorescence analysis) etc. analyze the content of metal contamination, first we need the metal contamination impurity of silicon chip surface to collect, current collection method is mainly carried out in two steps: first, the oxide-film on corrosion of silicon surface, makes silicon chip surface be hydrophobicity; Then, collect impurity by drop scanning method, produce sample to be analyzed.
The corrosion of silicon chip surface is the committed step of silicon slice surface sample preparation, and can affect the collection of next step sample to be analyzed, its principle is: utilize hydrofluoric acid (HF) and silicon chip surface oxide-film (SiO
2) reaction, and silicon (Si) itself is corroded hardly, reaction equation is: SiO
2+ 4HF=SiF
4↑+2H
2o.In corrosion process, the surface metal be attached on natural oxide film can be dissolved among the moisture film of Surface Creation, and silicon chip surface, also in hydrophobicity, has been convenient to the scanning of next step drop and has collected.
In practical operation, because the natural oxide film of some silicon chip surface is very thin, the epitaxial wafer especially just completed, does not almost have oxide-film, even if this just causes after HF corrosion process, still well cannot collect the sample of metallic contaminants from surface.Therefore, for such silicon chip, be necessary carrying out in corrosion process, first make its surface form dense oxidation film and corrode again, to facilitate the collection of follow-up middle metallic contaminants from surface.
Summary of the invention
The object of this invention is to provide a kind of surface treatment of silicon slice surface sample preparation and the technique of corrosion and device, this simple process, device is compact, easy to operate, is conducive to drop scanning method and collects impurity, produce sample to be analyzed.
For achieving the above object, the present invention by the following technical solutions:
Thisly to comprise the following steps for the surface treatment of silicon slice surface sample preparation and the technique of corrosion:
(1), by silicon chip put on the support column of corrosion device silicon wafer stage, then close the lid of corrosion cavity;
(2), ozone enters in the corrosion cavity of sealing, contacts with silicon chip surface, silicon chip surface is oxidized to fine and close oxide-film, and the valve (V5) of gas extraction system is opened simultaneously, and this process control is at 3-5 minute;
(3), with nitrogen, hydrofluoric acid steam fog is brought in corrosion cavity, lower the temperature below silicon wafer stage simultaneously, make HF steam fog at silicon chip surface congealing reaction, better eroded by oxide-film, excessive gas enters special sour discharge duct through steam vent (1-4);
(4), continue to pass into nitrogen in the corrosion cavity of sealing, in cavity, no longer include HF steam fog;
(5) lid, corroding cavity takes out silicon chip carries out silicon chip surface scanning and sample collection to next silicon chip scanning means.
This surface treatment for silicon slice surface sample preparation and corrosion device comprise: corrosion cavity (1), housing (2), be provided with silicon wafer stage (4) and logical ozone or nitrogen inlet (1-1) in cavity, by nitrogen as the HF gas access (1-2) of carrier and steam vent (1-4), also comprise the HF container (5) of peripheral hardware, the entrance (1-1) of logical ozone or nitrogen is connected in series valve V2, flow control valve MFC
1, MFC
1another termination threeway, a termination nitrogen pipeline of threeway, the outlet on another termination ozonizer road of threeway.
Ozone pipeline comprises ozone generator (6), and ozone generator is that oxygen forms the ozone generator of ozone through Ultraviolet radiation.
Described is provided with flow control valve MFC by nitrogen as in the HF gas inlet line of carrier
2and nitrogen pressure control valve V6.
In this corrosion device, corrosion cavity 1 and housing 2, HF container 5, and the part system of connected pipeline utilizes the existing device (model is: WSPSPAD-Fume producer: GeMeTec) of market sale.Ozone pipeline described in the utility model is connected to MFC in nitrogen pipeline
1hold an ozone pipeline in parallel.
First this device utilizes ozone (O
3) strong oxidizing property, rapidly silicon chip surface is formed fine and close oxide-film, then surface film oxide is effectively corroded, reach the object being convenient to the scanning of next step drop and sample collection.
Material used in the present invention all adopts the high-purity material meeting integrated circuit requirement, resistance to sour, and can not bring particle, metal contamination.As PTFE or macromolecule polyethylene material.Nitrogen and oxygen all adopt high-purity gas.
Advantage of the present invention is: first utilize ozone silicon chip surface first to be formed fine and close oxide-film, again surface film oxide is effectively corroded, and make silicon chip surface be hydrophobicity, so just be conducive to next step with the scanning of drop to silicon chip hydrophobic surface and the collection of metal impurities, simple process, apparatus structure is compact, easy to operate, effective.
Accompanying drawing explanation
Fig. 1: surface treatment provided by the invention and corrosion device schematic diagram
Fig. 2: Fig. 1 vertical view corroding cavity silicon wafer stage
Ozone generator schematic diagram in Fig. 3: Fig. 1
In Fig. 1, Fig. 2, Fig. 3,1 is corrosion cavity, and 2 is housing, 3 is the control arm of cover cap, 1-1 is ozone or the nitrogen inlet of cavity, and 1-2 is that 1-4 is steam vent by the HF gas access of nitrogen as carrier, 4 is silicon wafer stage, silicon wafer stage is provided with carrying silicon chip post 4-1 (totally 3), and 5 is HF container, and 6 is ozone generator, 6-1 is quartz burner, and V6 is nitrogen pressure control valve.V1, V2, V3, V4, V5 are valve, MFC
1, MFC
2for flow control valve, V7 is pressure reliability type valves.
Embodiment
This device comprises: corrosion cavity 1 and housing 2, cavity is provided with ozone or nitrogen inlet 1-1, by nitrogen as the HF gas access 1-2 of carrier and steam vent 1-4, silicon wafer stage 4.
The ozone used in the utility model is the method generation of common Ultraviolet radiation, adopts the fluorescent tube of the ultraviolet light of wavelength X=185nm, irradiates oxygen molecule (O
2) decompose and aggregate into ozone (O
3).Ozone enters in the corrosion cavity of sealing, contact with silicon chip surface, silicon chip surface is oxidized to fine and close oxide-film rapidly, and then with nitrogen, hydrofluoric acid (HF) steam fog is brought in corrosion cavity, lower the temperature below silicon wafer stage simultaneously, make HF steam fog can be good at, at silicon chip surface congealing reaction, better being eroded by oxide-film, enter special sour discharge duct more than gas through steam vent 1-4.Then continue to pass into nitrogen in the corrosion cavity of sealing, to guarantee to no longer include HF steam fog in cavity, the lid can opening corrosion cavity takes out silicon chip carries out silicon chip surface scanning and sample collection to next silicon chip scanning means.
Concrete operation step:
The first step: silicon chip is put on the support column of corrosion device silicon wafer stage, close the lid of corrosion cavity again, open valve V1, V2, oxygen is made to enter ozone generator, the ozone produced enters cavity through flow controller and valve V2, the valve V5 of gas extraction system opens simultaneously, and process control was at 3 to 5 minutes;
Second step: valve-off V1, V2, open valve V3, V4, make nitrogen through pressure-control valve and flow control, some enters in HF container, HF concentration is 38%, HF atomization is sent in corrosion cavity, another part is through the valve V3 of series connection, V4 brings the HF steam fog produced in HF container into cavity by the road, use common recirculated cooling water device to lower the temperature to silicon chip below silicon wafer stage simultaneously, thermostat is used temperature to be controlled at 14 DEG C-16 DEG C, time controling is between 10 minutes to 15 minutes, in the process, guarantee that total nitrogen pressure is not less than 1000hPa, meanwhile, due to the danger of HF, enter HF container place at nitrogen, fill a pressure reliability type valves V7, when this road nitrogen pressure is greater than 500hPa, automatically open, be exhausted (this step adopts existing model to be: this step in WSPSPAD-Fume equipment).
3rd step: valve-off V3, V4, opens valve V2, makes nitrogen continue to enter cavity, and discharged through steam vent by HF remaining in cavity, process control was at 6 to 8 minutes.Finally can open the lid of cavity, silicon chip extracting be carried out scanning and the sample collection of silicon chip surface to next silicon chip scanning means.
Claims (5)
1. one kind for the surface treatment of silicon slice surface sample preparation and the technique of corrosion: it is characterized in that: it comprises the following steps:
(1), by silicon chip put on the support column of corrosion device silicon wafer stage, then close the lid of corrosion cavity;
(2), ozone enters in the corrosion cavity of sealing, contacts with silicon chip surface, silicon chip surface is oxidized to fine and close oxide-film, and the valve (V5) of gas extraction system is opened simultaneously, and this process control is at 3-5 minute;
(3), with nitrogen, hydrofluoric acid steam fog is brought in corrosion cavity, lower the temperature below silicon wafer stage simultaneously, make HF steam fog at silicon chip surface congealing reaction, better eroded by oxide-film, excessive gas enters special sour discharge duct through steam vent (1-4);
(4), continue to pass into nitrogen in the corrosion cavity of sealing, in cavity, no longer include HF steam fog;
(5) lid, corroding cavity takes out silicon chip carries out silicon chip surface scanning and sample collection to next silicon chip scanning means.
2. a kind of surface treatment for silicon slice surface sample preparation according to claim 1 and etching process, is characterized in that: the temperature of cooling controls at 14 DEG C-16 DEG C, and time controling is between 10 minutes to 15 minutes.
3. the surface treatment for the silicon slice surface sample preparation of technique described in claim 1 and corrosion device, it comprises: corrosion cavity (1), housing (2), be provided with silicon wafer stage (4) and logical ozone or nitrogen inlet (1-1) in cavity, by nitrogen as the HF gas access (1-2) of carrier and steam vent (1-4), also comprise the HF container (5) of peripheral hardware, it is characterized in that: the entrance (1-1) of logical ozone or nitrogen is connected in series valve V2, flow control valve MFC
1, MFC
1another termination threeway, a termination nitrogen pipeline of threeway, the outlet on another termination ozonizer road of threeway.
4. a kind of surface treatment for silicon slice surface sample preparation according to claim 3 and corrosion device, it is characterized in that: ozone pipeline comprises ozone generator (6), ozone generator is that oxygen forms the ozone generator of ozone through Ultraviolet radiation.
5. a kind of surface treatment for silicon slice surface sample preparation according to claim 3 and corrosion device, is characterized in that: described is provided with flow control valve MFC by nitrogen as in the HF gas inlet line of carrier
2and nitrogen pressure control valve V6.
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| CN201110417124.6A CN103165407B (en) | 2011-12-14 | 2011-12-14 | A kind of for the surface treatment of silicon slice surface sample preparation and the technique of corrosion and device |
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| CN201110417124.6A CN103165407B (en) | 2011-12-14 | 2011-12-14 | A kind of for the surface treatment of silicon slice surface sample preparation and the technique of corrosion and device |
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| CN103165407B true CN103165407B (en) | 2016-04-06 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106298586A (en) * | 2015-06-04 | 2017-01-04 | 有研半导体材料有限公司 | A kind of silicon chip surface HF acid treatment system |
| CN106098597A (en) * | 2016-07-14 | 2016-11-09 | 江苏永能光伏科技有限公司 | A kind of closed ozone spraying system |
| CN107610998B (en) * | 2017-07-21 | 2020-09-15 | 江苏鲁汶仪器有限公司 | Gas phase corrosion cavity capable of adjusting internal and external pressure difference and method for gas phase corrosion by using same |
| CN107546145B (en) * | 2017-08-18 | 2020-12-29 | 清华大学 | Wafer in-situ detection device, wafer bracket and wafer in-situ detection method |
| CN107799446B (en) * | 2017-11-14 | 2023-07-14 | 扬州扬杰电子科技股份有限公司 | Cleaning device before chip potential barrier |
| CN113782465B (en) * | 2021-11-11 | 2022-02-18 | 西安奕斯伟材料科技有限公司 | Method for detecting metal on surface of wafer |
| CN117367924A (en) * | 2022-06-29 | 2024-01-09 | 江苏鲁汶仪器股份有限公司 | Metal contamination collection system and metal contamination collection method |
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Address after: 100088 Beijing city Xicheng District Xinjiekou Avenue No. 2 Applicant after: YOUYAN NEW MATERIAL CO., LTD. Address before: 100088 Beijing city Xicheng District Xinjiekou Avenue No. 2 Applicant before: GRINM Semiconductor Materials Co., Ltd. |
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Effective date of registration: 20150615 Address after: 101300 Beijing city Shunyi District Shuanghe Linhe Industrial Development Zone on the south side of the road Applicant after: You Yan Semi Materials Co., Ltd. Address before: 100088 Beijing city Xicheng District Xinjiekou Avenue No. 2 Applicant before: YOUYAN NEW MATERIAL CO., LTD. |
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Address after: 101300 south side of Shuanghe Road, Linhe Industrial Development Zone, Shunyi District, Beijing Patentee after: Youyan semiconductor silicon materials Co.,Ltd. Address before: 101300 south side of Shuanghe Road, Linhe Industrial Development Zone, Shunyi District, Beijing Patentee before: GRINM SEMICONDUCTOR MATERIALS Co.,Ltd. |
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