CN101850944B - Method for sedimentating silicon nitride thin film by using 13.56 MHz radio frequency power source - Google Patents
Method for sedimentating silicon nitride thin film by using 13.56 MHz radio frequency power source Download PDFInfo
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- CN101850944B CN101850944B CN2009100812249A CN200910081224A CN101850944B CN 101850944 B CN101850944 B CN 101850944B CN 2009100812249 A CN2009100812249 A CN 2009100812249A CN 200910081224 A CN200910081224 A CN 200910081224A CN 101850944 B CN101850944 B CN 101850944B
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- nitride film
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Abstract
The invention discloses a method for sedimentating a silicon nitride thin film by using a 13.56 MHz radio frequency power source. The method comprises the following steps of: firstly, cleaning and preheating a sample; secondly, sedimentating the silicon nitride thin film on the sample; and thirdly, annealing the sample sedimentated with the silicon nitride thin film. The invention only uses one power source, has simple and fast operation and strong universality, and can sedimetate the thin film more than 2 microns which has small stress and favorable corrosion resistance.
Description
Technical field
The present invention relates to the semiconductor film preparing technical field, particularly a kind of method that adopts 13.56MHz radio frequency power source deposit low stress nitride silicon film.
Background technology
Micro mechanical system (Micro Electro-Mechanical System is a kind of emerging little ME MEMS), mainly utilizes the mechanical property of material to make device, like transmitter, and micro motor, micro switch etc.
Silicon nitride film is a kind of physics and all very good dielectric film of chemical property; Has good insulation performance property, stability; Higher anti-oxidant, resistance to corrosion and excellent foreign ion and the advantages such as screening ability of steam, uses such as the final resist of Chang Zuowei, surface passivation layer in semiconducter device and unicircuit.Simultaneously; Silicon nitride film also has high firmness, high Young's modulus, good fatigue resistance, anti-good mechanics and the mechanical propertys such as ability and wear resistance that fracture; In the MEMS system, use also very extensively, be usually used in making structure units such as probe, socle girder.
The preparation method of silicon nitride film has a lot, but wherein mostly like low-pressure chemical vapor phase deposition (LPCVD) method, the pyroprocess of needs more than 700 ℃, and for must avoiding the pyritous device not meet the demands, and speed of response is also slower.Plasma enhanced CVD (Plasma-Enhanced Chemical Vapor Deposition; PECVD) has deposition temperature low (＜400 ℃); Deposition speed is fast, repeatability and good uniformity, advantage such as film defects density is lower and obtained extensive application.
At present, too high stress is that silicon nitride film prepares the outstanding problem in the process, surpasses certain thickness silicon nitride film and crack performance often occurs.And in the cantilever beam structures of MEMS system,, the stress in the film is required strict more because not do not support, otherwise structure will rupture or curl, and causes structural failure.Therefore, the preparation of the silicon nitride film of low-stress even zero stress is extremely important.
The most frequently used method of PECVD deposit low stress nitride silicon film is to use the dual band radio frequency source.It is generally acknowledged that the silicon nitride film that is higher than the radio frequency source deposit of 4MHz shows as tension stress usually, the film that is lower than the radio frequency source deposit of 4MHz shows as stress.Two frequency alternating depositions are controlled the film that final deposit goes out low-stress even zero stress through the time.But this method requirement equipment has two cover radio frequency sources, spends higher.And under a lot of situation, cantilever beam structures is to be combined by silicon nitride film and other materials, needs the size of counter stress to finely tune, and uses the method parameter of two cover radio frequency sources complicated, wayward.
In the MEMS system, the release of cantilever beam structures often needs the erosion removal sacrifice layer, therefore requires silicon nitride film that good corrosion resistance is arranged.As for the most frequently used silicon dioxide sacrificial layer, require silicon nitride that good anti-HF performance is arranged.
Summary of the invention
The technical problem that (one) will solve
In view of this; Main purpose of the present invention is to provide a kind of method of the 13.56MHz of employing radio frequency power source deposit low stress nitride silicon film; The 13.56MHz radio frequency power source that only uses general PECVD equipment all to be equipped with, deposit goes out the silicon nitride film of low-stress.
(2) technical scheme
For achieving the above object, the invention provides a kind of method of the 13.56MHz of employing radio frequency power source deposition silicon nitride film, this method comprises:
Step 1: sample is cleaned and preheating;
Step 2: deposition silicon nitride film on sample;
Step 3: the sample to being deposited with silicon nitride film is annealed.
In the such scheme; Said step 1 specifically comprises: sample is cleaned and dries up with nitrogen, put into plasma enhanced CVD PECVD Vakuumkammer, preheating 5 minutes; Make sample be warming up to 300 ℃ and also keep stable, remove steam residual in the sample simultaneously.
In the such scheme, said sample is Si sheet or quartz plate; For the Si sheet, sample is cleaned employing standard RCA cleaning, concrete cleaning step is: use No. 3 liquid H
2SO
4: H
2O
2Boiled 20 minutes more than=5: 1,90 ℃, washed with de-ionized water 5 minutes is used liquid NH then No. 1
3H
2O: H
2O
2: H
2O=1: 2: 5,80 ℃ were boiled 5 minutes, and washed with de-ionized water 5 minutes re-uses liquid HCl: H No. 2
2O
2: H
2O=1: 2: 7,80 ℃ were boiled 10 minutes, washed with de-ionized water 5 minutes, and using volume ratio at last is 10% HF aqueous solution soaking, washed with de-ionized water 10 minutes; For quartz plate, the concrete cleaning step that sample is cleaned is: acetone ultrasonic cleaning 5 minutes, absolute ethyl alcohol ultrasonic cleaning 3 minutes, deionized water ultrasonic cleaning 5 minutes.
In the such scheme, said step 2 specifically comprises: Vakuumkammer is evacuated to 10
-2Below the Pa, feed process gas, this process gas includes NH
3, N
2With volume ratio be 5% SiH
4, wherein, SiH
4Flow be 600～900sccm, NH
3Flow be 20～55sccm, N
2Flow be 1200～1960sccm; Air pressure remains on 70～120Pa, stablizes and adopts the radio frequency power build-up of luminance that is higher than 100W after 10 seconds, on sample, begins deposition silicon nitride film; Deposition time 25 minutes; Deposition thickness is the silicon nitride film more than 1 micron, and membrane stress is less than 50MPa, and film is HF: NH in volume ratio
4F: DI Water=1: the erosion rate in 2: 3 the BHF solution be 340～500 dusts/minute.
In the such scheme, said step 3 specifically comprises: adopt the annealing temperature more than 700 ℃ or 900 ℃, use lehre to anneal half a hour; Perhaps adopt the annealing temperature more than 700 ℃ or 900 ℃, used rapid thermal annealing 30 seconds.
In the such scheme, adopt 700 ℃ of annealing, erosion rate reduce to 102 dusts/minute, be original 25%.Adopt annealing more than 900 ℃, erosion rate reduce to 27 dusts/minute, be original 7%.
(3) beneficial effect
Can find out that from technique scheme the present invention has following beneficial effect:
1, the method for this employing 13.56MHz radio frequency power source deposit low stress nitride silicon film provided by the invention; The 13.56MHz radio frequency power source that only uses general PECVD equipment all to be equipped with just can deposit goes out the silicon nitride film of low-stress, method simple and fast; Universality is strong; But the film of deposit more than 2 microns, membrane stress is little, and corrosion resistance is good.
2, the method for this employing 13.56MHz radio frequency power source deposit low stress nitride silicon film provided by the invention, the compactness extent of film is very high, and is very excellent to the resistance to corrosion of HF.
3, the method for this employing 13.56MHz radio frequency power source deposit low stress nitride silicon film provided by the invention adopts the power build-up of luminance that is higher than 100W, improves the ionization level of gas molecule in the plasma body and the energy of various particles, makes its bombardment effect stronger.Strong bombardment effect help removing bonding force in the silicon nitride film more weak contain hydrogen group, make the stress deflection stress of film.Simultaneously, the film of deposit will be fine and close more, and corrosion resistance is better.
Description of drawings
Fig. 1 is the method flow diagram of employing 13.56MHz radio frequency power source deposit low stress nitride silicon film provided by the invention.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, to further explain of the present invention.
As shown in Figure 1, Fig. 1 is the method flow diagram of employing 13.56MHz radio frequency power source deposit low stress nitride silicon film provided by the invention, and this method may further comprise the steps:
Step 1: sample is cleaned and preheating.
In this step, sample is cleaned and dries up with nitrogen, put into plasma enhanced CVD (PECVD) Vakuumkammer, preheating 5 minutes makes sample be warming up to 300 ℃ and also keeps stable, removes steam residual in the sample simultaneously.Said sample is generally Si sheet or quartz plate.
If the Si sheet adopts standard RCA cleaning, concrete cleaning step is acetone ultrasonic cleaning 5 minutes, absolute ethyl alcohol ultrasonic cleaning 3 minutes, and washed with de-ionized water 5 minutes is used liquid H then No. 3
2SO
4: H
2O
2=5: 1,20 minute, washed with de-ionized water 5 minutes, No. 1 liquid NH
3H
2O: H
2O
2: H
2O=1: 1: 5,5 minutes, washed with de-ionized water 5 minutes, No. 2 liquid HCl: H
2O
2: H
2O=1: 1: 5,10 minutes, washed with de-ionized water 5 minutes, the HF aqueous solution soaking of using 10% volume ratio at last be after several seconds, washed with de-ionized water 10 minutes.
If quartz plate, concrete cleaning step is acetone ultrasonic cleaning 5 minutes, absolute ethyl alcohol ultrasonic cleaning 3 minutes, deionized water ultrasonic cleaning 5 minutes.
Step 2: deposition silicon nitride film on sample.
In this step, Vakuumkammer is evacuated to 10
-2Below the Pa, feed process gas, this process gas includes NH
3, N
2With volume ratio be 5% SiH
4, wherein, SiH
4Flow be 600～900sccm, NH
3Flow be 20～55sccm, N
2Flow be 1200～1960sccm; Air pressure remains on 70～120Pa, stablizes and adopts the radio frequency power build-up of luminance that is higher than 100W (adopting 150W in the present embodiment) after 10 seconds, on sample, begins deposition silicon nitride film; Deposition time 33 minutes; The silicon nitride film that deposit is 1.3 microns, membrane stress are stress 28MPa, at BHF (volume ratio HF: NH
4F: DI Water=1: 2: 3) erosion rate in the solution be 410 dusts/minute.
Step 3: the sample to being deposited with silicon nitride film is annealed.
Use lehre annealing half a hour, perhaps used rapid thermal annealing (RTP) 30 seconds, annealing temperature is more than 900 ℃, the BHF erosion rate reduce to 27 dusts/minute, be original 7%.If annealing temperature is 700 ℃, the HF erosion rate reduce to 102 dusts/minute, be original 25%.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a method that adopts 13.56MHz radio frequency power source deposition silicon nitride film is characterized in that, this method comprises:
Step 1: sample is cleaned and preheating;
Step 2: deposition silicon nitride film on sample;
Step 3: the sample to being deposited with silicon nitride film is annealed;
Wherein, said step 2 specifically comprises: Vakuumkammer is evacuated to 10
-2Below the Pa, feed process gas, this process gas includes NH
3, N
2With volume ratio be 5% SiH
4, wherein, SiH
4Flow be 600～900sccm, NH
3Flow be 20～55sccm, N
2Flow be 1200～1960sccm; Air pressure remains on 70～120Pa, stablizes and adopts the radio frequency power build-up of luminance that is higher than 100W after 10 seconds, on sample, begins deposition silicon nitride film; Deposition time 25 minutes; Deposition thickness is the silicon nitride film more than 1 micron, and membrane stress is less than 50MPa, and film is HF: NH in volume ratio
4F: DI Water=1: the erosion rate in 2: 3 the BHF solution be 340～500 dusts/minute.
2. the method for employing 13.56MHz radio frequency power source deposition silicon nitride film according to claim 1 is characterized in that said step 1 specifically comprises:
Sample is cleaned and dries up with nitrogen, put into plasma enhanced CVD PECVD Vakuumkammer, preheating 5 minutes makes sample be warming up to 300 ℃ and also keeps stable, removes steam residual in the sample simultaneously.
3. the method for employing 13.56MHz radio frequency power source deposition silicon nitride film according to claim 2 is characterized in that said sample is Si sheet or quartz plate;
For the Si sheet, sample is cleaned employing standard RCA cleaning, concrete cleaning step is: use No. 3 liquid H
2SO
4: H
2O
2Boiled 20 minutes more than=5: 1,90 ℃, washed with de-ionized water 5 minutes is used liquid NH then No. 1
3H
2O: H
2O
2: H
2O=1: 2: 5,80 ℃ were boiled 5 minutes, and washed with de-ionized water 5 minutes re-uses liquid HCl: H No. 2
2O
2: H
2O=1: 2: 7,80 ℃ were boiled 10 minutes, washed with de-ionized water 5 minutes, and using volume ratio at last is 10% HF aqueous solution soaking, washed with de-ionized water 10 minutes;
For quartz plate, the concrete cleaning step that sample is cleaned is: acetone ultrasonic cleaning 5 minutes, absolute ethyl alcohol ultrasonic cleaning 3 minutes, deionized water ultrasonic cleaning 5 minutes.
4. the method for employing 13.56MHz radio frequency power source deposition silicon nitride film according to claim 1 is characterized in that said step 3 specifically comprises:
Adopt 700 ℃ annealing temperature or adopt the annealing temperature more than 900 ℃, use lehre to anneal half a hour; Perhaps
Adopt 700 ℃ annealing temperature or adopt the annealing temperature more than 900 ℃, used rapid thermal annealing 30 seconds.
5. the method for employing according to claim 4 13.56MHz radio frequency power source deposition silicon nitride film is characterized in that, adopts 700 ℃ of annealing, erosion rate reduce to 102 dusts/minute.
6. the method for employing according to claim 4 13.56MHz radio frequency power source deposition silicon nitride film is characterized in that, adopts annealing more than 900 ℃, erosion rate reduce to 27 dusts/minute.
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| CN101850944B true CN101850944B (en) | 2012-03-28 |
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| CN102354664B (en) * | 2011-09-28 | 2015-12-16 | 上海华虹宏力半导体制造有限公司 | Intermetallic dielectric layer forming method and semiconductor device |
| CN102592974B (en) * | 2012-03-20 | 2014-07-02 | 中国科学院上海微系统与信息技术研究所 | Preparation method for high-K medium film |
| CN103855092B (en) * | 2012-11-28 | 2018-11-06 | 中国科学院微电子研究所 | Method, semi-conductor device manufacturing method |
| CN104143534B (en) * | 2013-05-10 | 2018-05-15 | 中国科学院微电子研究所 | Method, semi-conductor device manufacturing method |
| CN109216153B (en) * | 2017-07-03 | 2021-01-05 | 无锡华润上华科技有限公司 | Method for improving corrosion resistance of silicon nitride and preparation method of semiconductor device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609270A (en) * | 2004-11-16 | 2005-04-27 | 福州大学 | PECVD deposition low-tension SiN thin film technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609270A (en) * | 2004-11-16 | 2005-04-27 | 福州大学 | PECVD deposition low-tension SiN thin film technology |
Non-Patent Citations (3)
| Title |
|---|
| 李伟东等.PECVD氮化硅薄膜制备工艺研究.《中国机械工程》.2005,第16卷第396-398页. * |
| 杨景超等.PECVD中电子能量状态对氮化硅薄膜应力的影响.《新技术新工艺》.2007,(第7期),第102-104页. * |
| 陈玉武等.快速热处理对PECVD氮化硅薄膜性能的影响.《光电子·激光》.2008,第19卷(第10期),第1357-1360页. * |
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