CN109722645A - A kind of ultra-thin N doping carbon film and preparation method - Google Patents

A kind of ultra-thin N doping carbon film and preparation method Download PDF

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Publication number
CN109722645A
CN109722645A CN201811507849.2A CN201811507849A CN109722645A CN 109722645 A CN109722645 A CN 109722645A CN 201811507849 A CN201811507849 A CN 201811507849A CN 109722645 A CN109722645 A CN 109722645A
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thin
ultra
carbon film
preparation
doping carbon
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CN201811507849.2A
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郑学刚
李建褔
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Linyi University
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Linyi University
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Abstract

The invention belongs to thin film technique field, a kind of ultra-thin N doping carbon film and preparation method are disclosed, 20 grams of four ammoniums of hexa-methylene is accurately weighed, is added in silica crucible;Silicon wafer is put above, is placed in insulating box or crucible furnace and heats, and temperature is 250 degrees Celsius, and the time is 3 hours;Film sample is obtained above in silicon wafer, and sample is put into CVD furnace, is passed through nitrogen or ammonia, and at one atm, temperature is annealed 3~6 hours at 300~400 degrees Celsius, and silicon chip surface obtains ultra-thin N doping carbon film.Film thickness prepared by the present invention is at 10 nanometers hereinafter, N doping content is more than 20%.The preparation method of ultra-thin N doping carbon film provided by the invention, preparation process is simple, nontoxic, guarantees safety, while realizing that prepared by large area and production cost is low.

Description

A kind of ultra-thin N doping carbon film and preparation method
Technical field
The invention belongs to thin film technique field more particularly to a kind of ultra-thin N doping carbon film and preparation methods.
Background technique
Currently, the prior art commonly used in the trade is such that
Since with relatively high specific surface area, ultrathin carbon films are widely studied applied to fuel cell and micro- electricity in recent years Sub- technology, the application especially in composite material and function element can promote carbon-based nano electronics, Nano electro-mechanical system, And the development of nano biological sensor.Existing silicon-based semiconductor technique comparatively comparative maturity, if carbon film energy It is enough grown directly upon on silicon substrate, then will be very convenient when prepared by subsequent nano electron device and process.Doping is Adjust a kind of important method of carbon film band gap and conductive characteristic.If being able to use simple deposition technique, and can be directly in silicon The ultrathin carbon films of large area deposition severe N doping on substrate, then subsequent silicon substrate carbon nano electron device will be advantageous to Preparation.
In the prior art, ultrathin carbon films can use the method from top to bottom of chemical stripping, be prepared using blocky graphite, this Kind method includes the chemical reducing agent toxic to organism, is very restricted in production and living.More important is these changes Length of schooling Preparation Method with semiconductor device fabrication processes be it is unmatched, the carbon nanosheet of preparation be applied to need when prepared by device through It crosses in secondary transferring to silicon substrate, therefore cannot be directly compatible with silicon-based semiconductor technique.If it is what is removed with physical mechanical Words, it is difficult to large area preparation.Either chemical stripping or mechanical stripping are all difficult to prepare the carbon film of N doping.Ultrathin carbon films Can also with by it is lower and on evaporating deposition technique prepare, but equipment is expensive, technology complexity.Process may need to use high temperature ring Border, production cost are higher.
In conclusion problem of the existing technology is:
(1) either chemical stripping or mechanical stripping in the prior art, are all difficult to prepare the carbon film of N doping, and chemistry Removing includes the chemical reducing agent toxic to organism, is very restricted in production and living;Mechanical stripping is difficult to large area Preparation;
(2) ultrathin carbon films can also with by it is lower and on evaporating deposition technique prepare, but equipment is expensive, technology complexity; Process may need to use hot environment, and production cost is higher.
Solve the difficulty and meaning of above-mentioned technical problem: directly in grown above silicon ultrathin carbon films, there are no mature skills Art, is explored and to develop this technology significant for preparing micro-nano opto-electronic device.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of ultra-thin N doping carbon film and preparation methods.
The invention is realized in this way a kind of preparation method of ultra-thin N doping carbon film, specifically includes the following steps:
Step 1: 20 grams of four ammoniums of hexa-methylene are accurately weighed, are added in silica crucible;
Step 2: putting silicon wafer above, is placed in insulating box or crucible furnace and heats, and temperature is 250 degrees Celsius, and the time is 3 hours;
Step 3: film sample is obtained above in silicon wafer, and sample is put into CVD furnace, is passed through nitrogen or ammonia, big at one Under air pressure, temperature is annealed 3~6 hours at 300~400 degrees Celsius, obtains ultra-thin N doping carbon film in silicon chip surface.
Further, in step 1, four ammonium of hexa-methylene is that analysis is pure.
Another object of the present invention be to provide a kind of preparation method using the ultra-thin N doping carbon film prepare it is ultra-thin N doping carbon film, the ultra-thin N doping carbon film component is by mass content ratio by N 27.11%, C 69.48% and O 3.42% Composition.
Further, ultra-thin nitrogen-doped carbon film thickness described in the ultra-thin N doping carbon film is less than 10 nanometers.
Another object of the present invention is to provide a kind of fuel cell using the ultra-thin nitrogen-doped carbon film preparation.
It is raw that another object of the present invention is to provide a kind of utilize the ultra-thin nitrogen-doped carbon film preparation and microelectronics nanometer Object sensor.
In conclusion advantages of the present invention and good effect are as follows:
Film thickness prepared by the present invention is at 10 nanometers hereinafter, N doping content is more than 20%.Preparation provided by the invention The preparation process of method is simple, nontoxic, guarantees safety, while realizing that prepared by large area and production cost is low.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of ultra-thin N doping carbon film provided in an embodiment of the present invention.
Fig. 2 is the additive amount schematic diagram of ultra-thin N doping carbon film provided in an embodiment of the present invention.
Fig. 3 is ultra-thin N doping carbon film schematic diagram provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Application principle of the invention is described in detail with reference to the accompanying drawing.
As shown in Figure 1, the preparation method of ultra-thin N doping carbon film provided in an embodiment of the present invention, specifically includes following step It is rapid:
S101: 20 grams of four ammoniums of hexa-methylene are accurately weighed, are added in silica crucible;
S102: putting silicon wafer above, is placed in insulating box or crucible furnace and heats, and temperature is 250 degrees Celsius, the time 3 Hour;
S103: film sample is obtained above in silicon wafer, and sample is put into CVD furnace, is passed through nitrogen or ammonia, in an atmosphere Pressure, temperature are annealed 3~6 hours at 300~400 degrees Celsius, obtain ultra-thin N doping carbon film in silicon chip surface.
In step S101, four ammonium of hexa-methylene provided in an embodiment of the present invention is that analysis is pure.
In step S103, the film thickness of preparation provided in an embodiment of the present invention is at 10 nanometers hereinafter, N doping content is super Cross 20%.
As shown in Fig. 2, ultra-thin N doping carbon film additive amount schematic diagram provided in an embodiment of the present invention.
Ultra-thin N doping carbon film component provided by the invention is by mass content ratio by N 27.11%, C 69.48% and O 3.42% composition.
As shown in figure 3, the schematic diagram of ultra-thin N doping carbon film provided in an embodiment of the present invention.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (6)

1. a kind of preparation method of ultra-thin N doping carbon film, which is characterized in that the preparation method of the ultra-thin N doping carbon film, Specifically includes the following steps:
Step 1: four ammonium of hexa-methylene is accurately weighed, is added in silica crucible;
Step 2: putting silicon wafer above, is placed in insulating box or crucible furnace and heats, and temperature is 250 degrees Celsius, and the time is 3 small When;
Step 3: film sample is obtained above in silicon wafer, and sample is put into CVD furnace, is passed through nitrogen or ammonia, in an atmospheric pressure Under, temperature is annealed 3~6 hours at 300~400 degrees Celsius, obtains ultra-thin N doping carbon film in silicon chip surface.
2. the preparation method of ultra-thin N doping carbon film as described in claim 1, which is characterized in that in the step 1, six is sub- Four ammonium of methyl is that analysis is pure.
3. a kind of ultra-thin N doping carbon film prepared by the preparation method using ultra-thin N doping carbon film described in claim 1, special Sign is that the ultra-thin N doping carbon film component is made of by mass content ratio N 27.11%, C69.48% and O 3.42%.
4. ultra-thin N doping carbon film as claimed in claim 3, which is characterized in that ultra-thin nitrogen described in the ultra-thin N doping carbon film Doped carbon film thickness is less than 10 nanometers.
5. a kind of fuel cell using ultra-thin nitrogen-doped carbon film preparation described in claim 3.
6. it is a kind of using ultra-thin nitrogen-doped carbon film preparation described in claim 3 and microelectronics nano biological sensor.
CN201811507849.2A 2018-12-11 2018-12-11 A kind of ultra-thin N doping carbon film and preparation method Pending CN109722645A (en)

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CN201811507849.2A CN109722645A (en) 2018-12-11 2018-12-11 A kind of ultra-thin N doping carbon film and preparation method

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Application Number Priority Date Filing Date Title
CN201811507849.2A CN109722645A (en) 2018-12-11 2018-12-11 A kind of ultra-thin N doping carbon film and preparation method

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Application publication date: 20190507