CN106746711A - The method that ammonia reduction nitridation method prepares TiAlN thin film - Google Patents
The method that ammonia reduction nitridation method prepares TiAlN thin film Download PDFInfo
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- CN106746711A CN106746711A CN201611012115.8A CN201611012115A CN106746711A CN 106746711 A CN106746711 A CN 106746711A CN 201611012115 A CN201611012115 A CN 201611012115A CN 106746711 A CN106746711 A CN 106746711A
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- thin film
- tialn thin
- ammonia reduction
- tio
- film
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/225—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/281—Nitrides
Abstract
The present invention relates to TiAlN thin film preparing technical field, and in particular to a kind of method that ammonia reduction nitridation method prepares TiAlN thin film.The method that ammonia reduction nitridation method prepares TiAlN thin film, comprises the following steps：（1）Prepare TiO2Presoma；（2）Prepare TiAlN thin film.The present invention prepares TiAlN thin film by ammonia reduction-nitridation method, and the TiAlN thin film is NaCl type face-centered cubic TiN crystal, and film thickness is in 250 nm or so.TiAlN thin film not only has the optical characteristics similar with gold, also has the advantages that high rigidity, acid and alkali-resistance erosion, wear-resistant, high temperature resistant and good biocompatibility characteristics that other materials hardly match.
Description
Technical field
The present invention relates to TiAlN thin film preparing technical field, and in particular to a kind of ammonia reduction nitridation method prepares TiAlN thin film
Method.
Background technology
SERS (SERS) is a kind of highly sensitive spectral analysis technique having a high potential.Normal Raman spectrum
Method sensitivity is low, and SERS can provide the molecular signal adsorbed or near active substrate surface, so that
To more structural informations.The thus research of new and effective SERS active-substrate and preparation has turned into the weight of domestic and foreign scholars research
Point.Current preparation method is concentrated mainly on metal electrode, noble metal nano particles, film of roughening treatment etc..Using metal electricity
There is the defects such as pattern is uneven, stability is poor, cost is high as substrate in pole, noble metal nano particles.
The content of the invention
It is contemplated that regarding to the issue above, proposing a kind of method that ammonia reduction nitridation method prepares TiAlN thin film.The present invention
Technical scheme be：
The method that ammonia reduction nitridation method prepares TiAlN thin film, comprises the following steps：
（1）Prepare TiO2Presoma：
In vacuum glove box, measure 110 mL absolute ethyl alcohols and be put into wide-mouth bottle, add 10 mL titanium tetrachlorides, obtain four
Titanium chloride ethanol solution；Take 6 mL titanium tetrachlorides ethanol solutions and add beaker, add 10 mL anhydrous after being added thereto to 1g PVP
Ethanol and 2.5 mL DMF, are obtained TiO after dissolving2Precursor solution；
（2）Prepare TiAlN thin film：
With above-mentioned TiO2Precursor solution is titanium source, the plated film on quartz glass substrate, rotating speed be 3500 r/min, plated film 20s,
Then 24 h are heated at 80 DEG C and triggers non-hydrolytic gelation reaction, obtain TiO2Gel Precursor film, is warming up to 5 DEG C/min
400 DEG C, the min of pre-burning 30；
Repeat（2）3 times, common 3 layers of plated film；It is placed in tube-type atmosphere furnace, in the ammonia that flow is 800 mL/min, with 5 DEG C/
Min is warming up to 1000 DEG C of carbothermal reduction-nitridations and reacts 2 h, and TiAlN thin film is obtained after furnace cooling.
The described mL titanium tetrachlorides of addition 10 use pipette.
Described measuring when 110 mL absolute ethyl alcohols are put into wide-mouth bottle uses graduated cylinder.
Described uses sol evenning machine on quartz glass substrate during plated film.
The technical effects of the invention are that：
The present invention prepares TiAlN thin film by ammonia reduction-nitridation method, and the TiAlN thin film is NaCl type face-centered cubic TiN crystal, thin
Film thickness is in 250 nm or so.TiAlN thin film not only has the optical characteristics similar with gold, is also hardly matched with other materials
High rigidity, acid and alkali-resistance erosion, wear-resistant, high temperature resistant and good biocompatibility characteristics.
Specific embodiment
Embodiment 1
The method that ammonia reduction nitridation method prepares TiAlN thin film, comprises the following steps：
（1）Prepare TiO2Presoma：
In vacuum glove box, measure 110 mL absolute ethyl alcohols with graduated cylinder and be put into wide-mouth bottle, then 10 mL tetra- are added with pipette
Titanium chloride, obtains titanium tetrachloride ethanol solution；Take 6 mL titanium tetrachlorides ethanol solutions and add beaker, after being added thereto to 1g PVP
10 mL absolute ethyl alcohols and 2.5 mL DMF are added, TiO is obtained after dissolving2Precursor solution；
（2）Prepare TiAlN thin film：
With above-mentioned TiO2Precursor solution is titanium source, using sol evenning machine on quartz glass substrate plated film, rotating speed be 3500 r/
Min, plated film 20s, then heat 24 h and trigger non-hydrolytic gelation reaction at 80 DEG C, obtain TiO2Gel Precursor film, with 5
DEG C/min is warming up to 400 DEG C, the min of pre-burning 30；
Repeat（2）3 times, common 3 layers of plated film；It is placed in tube-type atmosphere furnace, in the ammonia that flow is 800 mL/min, with 5 DEG C/
Min is warming up to 1000 DEG C of carbothermal reduction-nitridations and reacts 2 h, and TiAlN thin film is obtained after furnace cooling.
Embodiment 2
The method that ammonia reduction nitridation method prepares TiAlN thin film, comprises the following steps：
（1）Prepare TiO2Presoma：
In vacuum glove box, measure 200 mL absolute ethyl alcohols with graduated cylinder and be put into wide-mouth bottle, then 20mL tetra- is added with pipette
Titanium chloride, obtains titanium tetrachloride ethanol solution；Take 5 mL titanium tetrachlorides ethanol solutions and add beaker, after being added thereto to 2g PVP
15mL absolute ethyl alcohols and 3 mL DMF are added, TiO is obtained after dissolving2Precursor solution；
（2）Prepare TiAlN thin film：
With above-mentioned TiO2Precursor solution is titanium source, using sol evenning machine on quartz glass substrate plated film, rotating speed be 4000 r/
Min, plated film 20s, then heat 24 h and trigger non-hydrolytic gelation reaction at 80 DEG C, obtain TiO2Gel Precursor film, with
10 DEG C/min is warming up to 400 DEG C, the min of pre-burning 30；
Repeat（2）3 times, common 4 layers of plated film；It is placed in tube-type atmosphere furnace, in the ammonia that flow is 1000 mL/min, with 5
DEG C/min is warming up to 1000 DEG C of carbothermal reduction-nitridations and reacts 2 h, and TiAlN thin film is obtained after furnace cooling.
Embodiment 3
The method that ammonia reduction nitridation method prepares TiAlN thin film, comprises the following steps：
（1）Prepare TiO2Presoma：
In vacuum glove box, measure 150 mL absolute ethyl alcohols with graduated cylinder and be put into wide-mouth bottle, then 20mL tetra- is added with pipette
Titanium chloride, obtains titanium tetrachloride ethanol solution；Take 8mL titanium tetrachlorides ethanol solution and add beaker, after being added thereto to 2g PVP
20mL absolute ethyl alcohols and 3 mL DMF are added, TiO is obtained after dissolving2Precursor solution；
（2）Prepare TiAlN thin film：
With above-mentioned TiO2Precursor solution is titanium source, using sol evenning machine on quartz glass substrate plated film, rotating speed be 4000 r/
Min, plated film 20s, then heat 24 h and trigger non-hydrolytic gelation reaction at 80 DEG C, obtain TiO2Gel Precursor film, with
10 DEG C/min is warming up to 400 DEG C, the min of pre-burning 30；
Repeat（2）3 times, common 3 layers of plated film；It is placed in tube-type atmosphere furnace, in the ammonia that flow is 1000 mL/min, with 5
DEG C/min is warming up to 1000 DEG C of carbothermal reduction-nitridations and reacts 2 h, and TiAlN thin film is obtained after furnace cooling.
The present invention prepares TiAlN thin film by ammonia reduction-nitridation method, and the TiAlN thin film is NaCl type face-centered cubics TiN brilliant
Body, film thickness is in 250 nm or so.TiAlN thin film not only has the optical characteristics similar with gold, is also difficult to other materials
The high rigidity of analogy, acid and alkali-resistance corrode, wear-resistant, high temperature resistant and good biocompatibility characteristics.
Claims (4)
1. the method that ammonia reduction nitridation method prepares TiAlN thin film, it is characterised in that：Comprise the following steps：
（1）Prepare TiO2Presoma：
In vacuum glove box, measure 110 mL absolute ethyl alcohols and be put into wide-mouth bottle, add 10 mL titanium tetrachlorides, obtain four
Titanium chloride ethanol solution；Take 6 mL titanium tetrachlorides ethanol solutions and add beaker, add 10 mL anhydrous after being added thereto to 1g PVP
Ethanol and 2.5 mL DMF, are obtained TiO after dissolving2Precursor solution；
（2）Prepare TiAlN thin film：
With above-mentioned TiO2Precursor solution is titanium source, the plated film on quartz glass substrate, rotating speed be 3500 r/min, plated film 20s,
Then 24 h are heated at 80 DEG C and triggers non-hydrolytic gelation reaction, obtain TiO2Gel Precursor film, is warming up to 5 DEG C/min
400 DEG C, the min of pre-burning 30；
Repeat（2）3 times, common 3 layers of plated film；It is placed in tube-type atmosphere furnace, in the ammonia that flow is 800 mL/min, with 5 DEG C/
Min is warming up to 1000 DEG C of carbothermal reduction-nitridations and reacts 2 h, and TiAlN thin film is obtained after furnace cooling.
2. the method that ammonia reduction nitridation method according to claim 1 prepares TiAlN thin film, it is characterised in that：Described adds
Enter 10 mL titanium tetrachlorides and use pipette.
3. the method that ammonia reduction nitridation method according to claim 1 prepares TiAlN thin film, it is characterised in that：Described amount
Take when 110 mL absolute ethyl alcohols are put into wide-mouth bottle and use graduated cylinder.
4. the method that ammonia reduction nitridation method according to claim 1 prepares TiAlN thin film, it is characterised in that：It is described
Sol evenning machine is used on quartz glass substrate during plated film.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325553A (en) * | 2018-02-02 | 2018-07-27 | 河南科技大学 | A kind of preparation method with the titanium nitride microspherical catalyst for coating core structure |
| CN109950047A (en) * | 2019-03-28 | 2019-06-28 | 西北工业大学 | The preparation method of the porous TiN electrode material of AMTEC |
| WO2019200599A1 (en) * | 2018-04-17 | 2019-10-24 | 中国科学院福建物质结构研究所 | Porous titanium nitride single crystal material, preparation method therefor and use thereof |
-
2016
- 2016-11-17 CN CN201611012115.8A patent/CN106746711A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325553A (en) * | 2018-02-02 | 2018-07-27 | 河南科技大学 | A kind of preparation method with the titanium nitride microspherical catalyst for coating core structure |
| WO2019200599A1 (en) * | 2018-04-17 | 2019-10-24 | 中国科学院福建物质结构研究所 | Porous titanium nitride single crystal material, preparation method therefor and use thereof |
| CN109950047A (en) * | 2019-03-28 | 2019-06-28 | 西北工业大学 | The preparation method of the porous TiN electrode material of AMTEC |
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