CN1631776A - Method for preparing silicide film by microwave hydrogen plasma - Google Patents
Method for preparing silicide film by microwave hydrogen plasma Download PDFInfo
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- CN1631776A CN1631776A CN 200410068036 CN200410068036A CN1631776A CN 1631776 A CN1631776 A CN 1631776A CN 200410068036 CN200410068036 CN 200410068036 CN 200410068036 A CN200410068036 A CN 200410068036A CN 1631776 A CN1631776 A CN 1631776A
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- microwave
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- hydrogen plasma
- hydrogen
- silicide film
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Abstract
The invention is a preparation method of metal silicide film by microwave hydrogen plasma, relates to film preparation field. The invention initiates solid phase reaction between metal film of nano-thickness and silicon base by processing them with microwave hydrogen plasma. First previously accumulate the nano-thickness on the silicon base and put the base into the reaction room of the microwave heating device. Aerate the reaction room with hydrogen after evacuation to provide a protective reducibility circumstance and generate heat plasma. The microwave is fed-in from the top of the reaction room so to generate hydrogen plasma. The temperature of the silicon base is controlled by adjusting the capacity of microwave and measured by external thermoscope through the quartz window so to stabilize the temperature by adjust the capacity of the microwave when the temperature reaches the set value. Acted by both hyperthermia of the plasma and microwave the metal film and the silicon base together solid phase reacts to get the metal silicide film.
Description
Technical field
The present invention relates to a kind of method for preparing metal silicide film, specifically is a kind of method of preparing silicide film by microwave hydrogen plasma.Be used for the film preparation field.
Background technology
Microwave is a kind of frequency electromagnetic waves, and its range of frequency is 0.3～300GHz.Microwave heating is to utilize the dielectric loss of dielectric medium in high-frequency electric field, and micro-wave energy is converted into heat energy.The microwave plasma heating then is to utilize rarefied gas ionization in the higher frequency electromagnetic field to produce plasma body glow discharge, and micro-wave energy is transformed into heat energy.Place the solid state medium of microwave plasma, not only be subjected to plasma body under the high-strength microwave electric field effect, make it rapid intensification, also be subjected to the direct irradiation of microwave electromagnetic field inevitably, and may have influence on its physico-chemical property the bombardment of dielectric surface.
Find that by prior art documents patent of invention 96115436.5 can reduce sintering temperature, shorten sintering time, improve ceramic performance etc.But notion metal traditionally is a microwave reflection, rather than can directly absorb microwave as pottery electromagnetic energy is converted into heat energy.Therefore the thermal treatment that microwave is used for metal is seldom arranged, also do not see the report that microwave is used to prepare metal silicide film.But when the thickness of metallic film entered into nanoscale, metallic film was not very serious to the reflection of microwave, and part or most of microwave can see through metallic film and propagate, and directly arrive at metallic film and substrate at the interface.On the other hand, microwave field can be in rarefied gas activated plasma, the metallic membrane and the substrate that are immersed in are wherein heated up rapidly.The two all will promote the solid state reaction between metallic membrane and the substrate.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, propose a kind of method of preparing silicide film by microwave hydrogen plasma.Make its metal silicide film that can prepare nanometer grade thickness apace, in large area, compatible mutually with the semiconductor microactuator electronic technology, and can prevent the oxidation of metallic film effectively.
The present invention is achieved by the following technical solutions; the present invention makes the metallic film of nanometer grade thickness and silicon substrate realize that solid state reaction prepares metal silicide film with microwave hydrogen plasma thermal treatment; at first with the metallic film pre-deposition of nano metal level thickness on silicon substrate; and place the reaction chamber of microwave heating installation; after vacuumizing, reaction chamber charges into hydrogen; be used to produce heating plasma and restitutive protection's atmosphere; microwave is by the top feed-in of reaction chamber and produce hydrogen plasma then; the silicon substrate temperature is by regulating microwave power control; and see through the quartz window be positioned at the reaction chamber upper lateral part by outside infrared thermometer and measure; after temperature reaches set(ting)value; regulate microwave power; make temperature reach stable; metallic film and silicon substrate carry out solid state reaction under the dual function of plasma high-temperature and microwave, form metal silicide film.
The present invention is applicable to iron (Fe), cobalt (Co), nickel (Ni), titanium (Ti), the film preparation of tungsten (W) refractory metal silicide, and the thickness of its metallic membrane is less than 100 nanometers.
The present invention's microwave of feed-in in reaction chamber is the microwave of 2.45GHz.Its role is to: 1. the microwave of 2.45GHz is easy to form Low Temperature Hydrogen Plasma in given nitrogen atmosphere.2. the microwave of 2.45GHz has higher transmittance in the metallic film less than 100 nano thickness, and microwave can see through the interface that metallic film acts directly on metal and silicon substrate.
After the reaction chamber of the present invention in device vacuumizes, charge into a certain amount of hydrogen.Its role is to: 1. produce hydrogen plasma, with the heating silicon substrate.2. in reaction chamber, form restitutive protection's atmosphere, to prevent burning.3. the high thermal conductivity of hydrogen is beneficial to that silicon substrate heats quickly and evenly and fast cooling.Reaction chamber base vacuum degree is higher than 1 * 10
-3Pa, the pressure that charges into hydrogen is 0.5 ~ 5kPa.
The metallic film that is deposited on the silicon substrate must well be protected before thermal treatment, prevented the oxidized or pollution in active metal.Silicon need place on the quartz holder, makes sample deposit the metal one side over against the thermometric window, to realize infrared measurement of temperature.The homogeneity that argon-arc plasma field should be avoided having influence in quartz holder structure of using and position as far as possible.Infrared thermometer is adjusted the slin emissivity parameter according to film kind and surface irregularity state in advance.
Temperature rise rate and thermostat temperature all can be regulated by microwave power, the temperature rise rate that different microwave powers is corresponding different.In the constant temperature stage, but microwave power also should keep adjustment state to guarantee the stable of temperature.
Close microwave source and can realize rapid cooling, also can strengthen feeding amounts of hydrogen or other supplementary means in addition and improve cooling rate.
In the present invention, sample is immersed in the microwave hydrogen plasma, under the dual function of hydrogen plasma thermal field and microwave electromagnetic field, carries out the method that the chemical impellent of solid state reaction heats more merely between metallic film and the silicon substrate and strengthens widely.Help improving speed of response, reduce temperature of reaction.And help the generation of the stable state phase of metal silicide.
Embodiment
Content in conjunction with the inventive method provides following examples:
Embodiment 1 microwave hydrogen plasma thermal treatment prepares the Ti-Si compound metal titanium that sputter 100nm is thick on silicon substrate (Ti) film, and the microwave reaction chamber is evacuated to 1 * 10
-3Pa charges into the hydrogen of 3kPa pressure.From the microwave of reactor top feed-in 2.45GHz, behind the hydrogen plasma build-up of luminance, temperature is raised to 800 ℃ in 10 seconds, constant temperature 3 minutes.Close microwave source, the rising hydrogen pressure is to 25kPa, and silicon substrate is cooled to room temperature rapidly.The square resistance of reaction rear film drops to 8.5 Ω/ from reacting preceding 70 Ω/, and X light diffracting analysis shows, has generated the TiSi of C54 phase after the microwave hydrogen plasma thermal treatment
2Compound.
Embodiment 2 microwave hydrogen plasma thermal treatments prepare the Co-Si compound
The cobalt metal that sputter 80nm is thick on silicon substrate (Co) film, the microwave reaction chamber is evacuated to 1 * 10
-3Pa charges into the hydrogen of 5kPa pressure.From the microwave of reactor top feed-in 2.45GHz, behind the hydrogen plasma build-up of luminance, 600 ℃ of constant temperature 3 minutes.Close microwave source, the rising hydrogen pressure is to 25kPa, and silicon substrate is cooled to room temperature rapidly.The square resistance of reaction rear film drops to 2.6 Ω/ from reacting preceding 10 Ω/, and X light diffracting analysis shows, has generated CoSi after the microwave hydrogen plasma thermal treatment
2Many silicon compounds.This is than under simple heat-treat condition, many silicon compounds CoSi
2Formation temperature low 50-100 ℃.And there is not transitional form Co
2The at first formation of Si and CoSi.Microwave hydrogen plasma thermal treatment has promoted many silicon stable phase CoSi
2Formation.
Embodiment 3 microwave hydrogen plasma thermal treatments prepare the Ni-Si compound
The metallic nickel that sputter 100nm is thick on silicon substrate (Ni) film, the microwave reaction chamber is evacuated to 1 * 10
-3Pa charges into the hydrogen of 0.5kPa pressure.From the microwave of reactor top feed-in 2.45GHz, behind the hydrogen plasma build-up of luminance, 500 ℃ of constant temperature 3 minutes.Close microwave source, the rising hydrogen pressure is to 25kPa, and silicon substrate is cooled to room temperature rapidly.X light diffracting analysis shows, has generated NiSi after the microwave hydrogen plasma thermal treatment
2Many silicon compounds.In the thermal treatment of routine, NiSi
2Just occur at the high temperature more than 700 ℃, microwave annealing thermal treatment makes NiSi
2Just directly formed at 500 ℃, and do not had transitional form Ni
2The at first formation of Si and NiSi.Microwave hydrogen plasma thermal treatment has promoted many silicon stable phase NiSi
2Formation.
Claims (4)
1; a kind of method of preparing silicide film by microwave hydrogen plasma; it is characterized in that; make the metallic film of nanometer grade thickness and silicon substrate realize that solid state reaction prepares metal silicide film with microwave hydrogen plasma thermal treatment; at first with the metallic film pre-deposition of nanometer grade thickness on silicon substrate; and place the reaction chamber of microwave heating installation; after vacuumizing, reaction chamber charges into hydrogen; be used to produce heating plasma and restitutive protection's atmosphere; microwave is by the top feed-in of reaction chamber and produce hydrogen plasma then; the silicon substrate temperature is by regulating microwave power control; and see through quartz window by outside infrared thermometer and measure; after temperature reaches set(ting)value; regulate microwave power; make temperature reach stable; metallic film and silicon substrate carry out solid state reaction under the dual function of plasma high-temperature and microwave, form metal silicide film.
2, the method for preparing silicide film by microwave hydrogen plasma according to claim 1 is characterized in that, is applicable to iron, cobalt, nickel, titanium, the film preparation of tungsten refractory metal silicide, and the thickness of its metallic membrane is less than 100 nanometers.
3, the method for preparing silicide film by microwave hydrogen plasma according to claim 1 is characterized in that, after the reaction chamber in device vacuumizes, charges into hydrogen, and reaction chamber base vacuum degree is higher than 1 * 10
-3Pa, the pressure that charges into hydrogen is 0.5 ~ 5kPa.
4, the method for preparing silicide film by microwave hydrogen plasma according to claim 1 is characterized in that, the microwave of feed-in is the microwave of 2.45GHz in reaction chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410068036 CN1631776A (en) | 2004-11-11 | 2004-11-11 | Method for preparing silicide film by microwave hydrogen plasma |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410068036 CN1631776A (en) | 2004-11-11 | 2004-11-11 | Method for preparing silicide film by microwave hydrogen plasma |
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| CN1631776A true CN1631776A (en) | 2005-06-29 |
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| CN 200410068036 Pending CN1631776A (en) | 2004-11-11 | 2004-11-11 | Method for preparing silicide film by microwave hydrogen plasma |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220469B (en) * | 2006-11-10 | 2010-08-11 | 肖特股份公司 | Method and apparatus for plasma enhanced chemical vapor deposition |
| CN105518830A (en) * | 2014-04-18 | 2016-04-20 | 富士电机株式会社 | Method for manufacturing semiconductor device |
| CN105518829A (en) * | 2014-04-18 | 2016-04-20 | 富士电机株式会社 | Method for manufacturing semiconductor device |
| CN105593975A (en) * | 2014-04-18 | 2016-05-18 | 富士电机株式会社 | Method for manufacturing semiconductor device |
-
2004
- 2004-11-11 CN CN 200410068036 patent/CN1631776A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220469B (en) * | 2006-11-10 | 2010-08-11 | 肖特股份公司 | Method and apparatus for plasma enhanced chemical vapor deposition |
| US7947337B2 (en) | 2006-11-10 | 2011-05-24 | Schott Ag | Method and apparatus for plasma enhanced chemical vapor deposition |
| CN105518830A (en) * | 2014-04-18 | 2016-04-20 | 富士电机株式会社 | Method for manufacturing semiconductor device |
| CN105518829A (en) * | 2014-04-18 | 2016-04-20 | 富士电机株式会社 | Method for manufacturing semiconductor device |
| CN105593975A (en) * | 2014-04-18 | 2016-05-18 | 富士电机株式会社 | Method for manufacturing semiconductor device |
| CN105518829B (en) * | 2014-04-18 | 2018-01-26 | 富士电机株式会社 | The manufacture method of semiconductor device |
| CN105518830B (en) * | 2014-04-18 | 2018-01-26 | 富士电机株式会社 | The manufacture method of semiconductor device |
| CN105593975B (en) * | 2014-04-18 | 2018-05-08 | 富士电机株式会社 | The manufacture method of semiconductor device |
| US9972499B2 (en) | 2014-04-18 | 2018-05-15 | Fuji Electric Co., Ltd. | Method for forming metal-semiconductor alloy using hydrogen plasma |
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