CN103165407A - Technology and device for surface treatment and corrosion of silicon slice surface sample preparation - Google Patents
Technology and device for surface treatment and corrosion of silicon slice surface sample preparation Download PDFInfo
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- CN103165407A CN103165407A CN2011104171246A CN201110417124A CN103165407A CN 103165407 A CN103165407 A CN 103165407A CN 2011104171246 A CN2011104171246 A CN 2011104171246A CN 201110417124 A CN201110417124 A CN 201110417124A CN 103165407 A CN103165407 A CN 103165407A
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Abstract
Disclosed are a technology for surface treatment and corrosion of silicon slice surface sample preparation and a device for the surface treatment and corrosion of the silicon slice surface sample preparation. The technology contains a process that ozone enters into a sealed corrosion cavity to contact with the surface of a silicon slice, so that the surface of the silicon slice is oxidized into a dense oxidation film. The device comprises the corrosion cavity (1) and a cover shade (2), wherein the cavity is provided with a silicon slice platform (4), an ozone or nitrogen leading inlet (1-1), an HF gas inlet (1-2) with nitrogen as a carrier, and an air discharge port (1-4), and further comprises an externally-arranged HF container (5). The ozone or nitrogen leading inlet (1-1) is in series connection with a valve V2 and a flow adjusting valve MFC1, the other end of the MFC1 is connected with a tee joint, one end of the tee joint is connected with a nitrogen pipeline, and the other end of the tee joint is connected with an outlet of the nitrogen pipeline. The technology and the device have the advantages that the ozone can be utilized for enabling the dense oxidation film to be first formed on the surface of the silicon slice, effective corrosion is conducted on the surface of the oxidation film, the surface of the silicon slice is enabled to have hydrophobic property, the process that liquid drop is used for scanning to the hydrophobic surface of the silicon slice in next step and collecting metal impurities is benefited, the process is simple and convenient to conduct, the structure of the device is compact, operation is easy, and effect is good.
Description
Technical field
The present invention relates to a kind of improvement of etching process and device of silicon chip surface sample preparation, be particularly useful for the silicon chip that the surface only has natural oxide film.
Background technology
Silicon chip is most popular backing material in integrated circuit, have in semi-conductive processing technology that to surpass 50% finished product loss late be that pollution by silicon face causes, be accompanied by the raising day by day of circuit level, the 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 defective (Haze). therefore, we need to carry out metal contamination test to silicon chip, and purpose is whether in allowed limits to confirm on silicon chip metal contamination, enter in subsequently procedure to avoid defective item.
Before using ICP-MS (inductivity coupled plasma mass spectrometry analysis), TXRF (x-ray fluorescence analysis) etc. that the content of metal contamination is analyzed, at first we need the metal contamination impurity of silicon chip surface is collected, present collection method is mainly carried out in two steps: at first, the oxide-film on corrosion of silicon surface makes silicon chip surface be hydrophobicity; Then, collect impurity by the drop scanning method, produce sample to be analyzed.
The corrosion of silicon chip surface is the committed step of silicon chip surface sample preparation, can affect the collection of next step sample to be analyzed, and 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 that is attached on natural oxide film can be dissolved among the moisture film of Surface Creation, and silicon chip surface also is hydrophobicity, has been convenient to next step drop scanning and has collected.
In practical operation, due to the natural oxide film of some silicon chip surface as thin as a wafer, the epitaxial wafer of especially just having completed does not almost have oxide-film, even this just causes through after the HF corrosion process, still can't well collect the sample of metallic contaminants from surface.Therefore, for such silicon chip, be necessary in carrying out corrosion process, first make its surface form dense oxidation film and corrode again, with the collection of convenient follow-up middle metallic contaminants from surface.
Summary of the invention
The technique and the device that the purpose of this invention is to provide a kind of surface treatment and corrosion of silicon chip surface sample preparation, this simple process, device is compact, and is easy to operate, is conducive to the drop scanning method and collects impurity, produces sample to be analyzed.
For achieving the above object, the present invention by the following technical solutions:
Thisly comprise the following steps for the surface treatment of silicon chip surface sample preparation and the technique of corrosion:
(1), silicon chip is put on the support column of corrosion device silicon wafer stage, then close the corrosion cavity lid;
(2), ozone enters in the corrosion cavity of sealing, contacts with silicon chip surface, and silicon chip surface is oxidized to fine and close oxide-film, opens the valve (V5) of gas extraction system;
(3), with nitrogen, the hydrofluoric acid steam fog is brought in the corrosion cavity, the silicon wafer stage below lowers the temperature simultaneously, make the HF steam fog at the silicon chip surface congealing reaction, better oxide-film is eroded, unnecessary gas enters special sour discharge duct through steam vent (1-4);
(4), continue to pass into nitrogen in the corrosion cavity of sealing, no longer include the HF steam fog in cavity;
(5), the lid taking-up silicon chip of corrosion cavity carries out scanning and the sample collection of silicon chip surface to next silicon chip scanning means.
This surface treatment and corrosion device for the silicon chip surface sample preparation comprises: corrosion cavity (1), housing (2), be provided with silicon wafer stage (4) and logical ozone or nitrogen inlet (1-1) in cavity, by HF gas access (1-2) and the exhaust outlet (1-4) of nitrogen as carrier, the HF container (5) that also comprises peripheral hardware, entrance (1-1) serial connection valve V2, the flow control valve MFC of logical ozone or nitrogen
1, MFC
1Another termination threeway, a termination nitrogen pipeline of threeway, the outlet on another termination ozonizer road of threeway.
The ozone pipeline comprises ozone generator (6), and ozone generator is that oxygen forms the ozone generator of ozone through the ultraviolet ray irradiation.
Described by being provided with flow control valve MFC in the HF gas access pipeline of nitrogen as carrier
2And nitrogen pressure control valve V6.
In this corrosion device, corrosion cavity 1 and housing 2, HF container 5, and the part of connected pipeline system utilizes the existing device of market sale, and (model is: WSPS PAD-Fume producer: GeMeTec).Ozone pipeline described in the present invention is to be connected to MFC in nitrogen pipeline
1Hold an ozone pipeline in parallel.
At 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 purpose of being convenient to next step drop scanning and sample collection.
Material used in the present invention all adopts the high-purity material that meets the integrated circuit requirement, acidproof corruption, 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 that silicon chip surface is first 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 drop to the scanning of silicon chip hydrophobic surface and the collection of metal impurities, simple process, apparatus structure is compact, and is easy to operate, effective.
Description of drawings
Fig. 1: surface treatment provided by the invention and corrosion device schematic diagram
Fig. 2: Fig. 1 corrodes the vertical view of cavity silicon wafer stage
Fig. 3: the ozone generator schematic diagram in Fig. 1
In Fig. 1, Fig. 2, Fig. 3,1 is the 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 exhaust outlet 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 the HF container, and 6 is ozone generator, 6-1 is quartz burner, and V6 is the nitrogen pressure control valve.V1, V2, V3, V4, V5 are valve, MFC
1, MFC
2Be flow control valve, V7 is pressure reliability valve.
Embodiment
This device comprises: corrosion cavity 1 and housing 2, cavity be provided with ozone or nitrogen inlet 1-1, by HF gas access 1-2 and the exhaust outlet 1-4 of nitrogen as carrier, silicon wafer stage 4.
The ozone that uses in the present invention is that the method that common ultraviolet ray is shone produces, and adopts the fluorescent tube of the ultraviolet light of wavelength X=185nm, irradiation oxygen molecule (O
2) decompose and aggregate into ozone (O
3).Ozone enters in the corrosion cavity of sealing, contact with silicon chip surface, rapidly silicon chip surface is oxidized to fine and close oxide-film, and then with nitrogen, hydrofluoric acid (HF) steam fog is brought in the corrosion cavity, the silicon wafer stage below lowers the temperature simultaneously, make the HF steam fog can be good at better oxide-film being eroded at the silicon chip surface congealing reaction, 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 the no longer including HF steam fog in cavity, the lid that can open the corrosion cavity takes out silicon chip and carries out scanning and the sample collection of silicon chip surface 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 again the lid of corrosion cavity, open valve V1, V2, make oxygen enter ozone generator, the ozone that produces 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 the HF container, HF concentration is 38%, the HF atomizing is sent in the corrosion cavity, another part is through the valve V3 of series connection, V4 brings the HF steam fog that produces in the HF container into cavity by the road, the silicon wafer stage below uses common recirculated cooling water device that silicon chip is lowered the temperature simultaneously, use thermostat that temperature is controlled at 14 ℃-16 ℃, time is controlled between 10 minutes to 15 minutes, in this process, guarantee that total nitrogen pressure is not less than 1000hPa, simultaneously, due to the danger of HF, enter HF container place at nitrogen, fill a pressure reliability valve V7,, automatically open during greater than 500hPa when this road nitrogen pressure, (this step adopts existing model to be: this step in WSPS PAD-Fume equipment) to carry out exhaust.
The 3rd step: valve-off V3, V4, open valve V2, make nitrogen continue to enter cavity, HF remaining in cavity to be discharged through steam vent, process control got final product at 6 to 8 minutes.The lid of cavity be can open at last, scanning and the sample collection of silicon chip surface silicon chip extracting carried out to next silicon chip scanning means.
Claims (5)
1. one kind is used for the surface treatment of silicon chip surface sample preparation and the technique of corrosion: it is characterized in that: it comprises the following steps:
(1), silicon chip is put on the support column of corrosion device silicon wafer stage, then close the corrosion cavity lid;
(2), ozone enters in the corrosion cavity of sealing, contacts with silicon chip surface, and silicon chip surface is oxidized to fine and close oxide-film, opens the valve (V5) of gas extraction system;
(3), with nitrogen, the hydrofluoric acid steam fog is brought in the corrosion cavity, the silicon wafer stage below lowers the temperature simultaneously, make the HF steam fog at the silicon chip surface congealing reaction, better oxide-film is eroded, unnecessary gas enters special sour discharge duct through steam vent (1-4);
(4), continue to pass into nitrogen in the corrosion cavity of sealing, no longer include the HF steam fog in cavity;
(5), the lid taking-up silicon chip of corrosion cavity carries out scanning and the sample collection of silicon chip surface to next silicon chip scanning means.
2. a kind of surface treatment and etching process for the silicon chip surface sample preparation according to claim 1, it is characterized in that: the temperature of cooling is controlled at 14 ℃-16 ℃, and the time is controlled between 10 minutes to 15 minutes.
3. surface treatment and corrosion device that is used for the silicon chip surface sample preparation of the described technique of claim 1, 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 HF gas access (1-2) and the exhaust outlet (1-4) of nitrogen as carrier, also comprise the HF container (5) of peripheral hardware, it is characterized in that: entrance (1-1) serial connection valve V2, the flow control valve MFC of logical ozone or nitrogen
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 and corrosion device for the silicon chip surface sample preparation according to claim 3, it is characterized in that: the ozone pipeline comprises ozone generator (6), ozone generator is that oxygen forms the ozone generator of ozone through the ultraviolet ray irradiation.
5. a kind of surface treatment and corrosion device for the silicon chip surface sample preparation according to claim 3 is characterized in that: described by being provided with flow control valve MFC in the HF gas access pipeline of nitrogen as 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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| CN103165407B CN103165407B (en) | 2016-04-06 |
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Cited By (7)
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| 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 |
| 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 |
| CN107546145A (en) * | 2017-08-18 | 2018-01-05 | 清华大学 | Wafer is in level detecting apparatus, wafer bracket and wafer in position detecting method |
| CN107610998A (en) * | 2017-07-21 | 2018-01-19 | 江苏鲁汶仪器有限公司 | A kind of gaseous corrosion cavity that can adjust inside and outside differential pressure and the method using its progress gaseous corrosion |
| CN107799446A (en) * | 2017-11-14 | 2018-03-13 | 扬州扬杰电子科技股份有限公司 | Cleaning device and cleaning before a kind of chip potential barrier |
| CN113782465A (en) * | 2021-11-11 | 2021-12-10 | 西安奕斯伟材料科技有限公司 | Method for detecting metal on surface of wafer |
| WO2024001081A1 (en) * | 2022-06-29 | 2024-01-04 | 江苏鲁汶仪器股份有限公司 | Metal contamination collecting system and metal contamination collecting method |
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| CN107610998A (en) * | 2017-07-21 | 2018-01-19 | 江苏鲁汶仪器有限公司 | A kind of gaseous corrosion cavity that can adjust inside and outside differential pressure and the method using its progress gaseous corrosion |
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| CN113782465A (en) * | 2021-11-11 | 2021-12-10 | 西安奕斯伟材料科技有限公司 | Method for detecting metal on surface of wafer |
| WO2024001081A1 (en) * | 2022-06-29 | 2024-01-04 | 江苏鲁汶仪器股份有限公司 | Metal contamination collecting system and metal contamination collecting method |
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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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