阅读说明：本技术 一种氮氧化钛薄膜及其基于激光剥离技术的制备方法 (A kind of titanium oxynitrides film and its preparation method based on laser lift-off technique ) 是由 洪瑞金 师境奇 张大伟 颜廷贞 李正旺 陶春先 于 2019-09-12 设计创作，主要内容包括：本发明提供一种氮氧化钛薄膜及其基于激光剥离技术的制备方法,包括：步骤1,将氮化钛陶瓷片放置到实验平台上,然后将洁净的玻璃基片放置到氮化钛陶瓷片上,使玻璃基片的下表面与氮化钛陶瓷片完全且紧密贴合；步骤2,采用脉冲激光器发出激光功率为2W,扫描速率为400mm/s的激光,将氮化钛颗粒从氮化钛陶瓷片上剥离到玻璃基片的表面且氮化钛颗粒与氧元素结合,得到附着在玻璃基片下面的氮氧化钛膜层；步骤3,采用脉冲激光器发出激光功率为2W,扫描速率为400mm/s或700mm/s的激光对氮氧化钛膜层进行辐照,得到氮氧元素含量得到改变的氮氧化钛薄膜。本发明的方法操作简单,成本低廉,且制备得到的氮氧化钛薄膜具有不错的热稳定性和附着力。(The present invention provides a kind of titanium oxynitrides film and its preparation method based on laser lift-off technique, it include: step 1, titanium nitride ceramic piece is placed on experiment porch, then clean glass substrate is placed into titanium nitride ceramic on piece, keeps the lower surface of glass substrate complete with titanium nitride ceramic piece and fitted closely；Step 2, pulse laser is used to issue laser power as 2W, sweep speed is the laser of 400mm/s, and the surface and titanium nitride particles by titanium nitride particles from the removing of titanium nitride ceramic on piece to glass substrate obtain being attached to the titanium oxynitrides film layer below glass substrate in conjunction with oxygen element；Step 3, pulse laser is used to issue laser power as 2W, sweep speed is that the laser of 400mm/s or 700mm/s irradiates titanium oxynitrides film layer, obtains the titanium oxynitrides film that nitrogen oxygen element content is changed.Method of the invention is easy to operate, low in cost, and the titanium oxynitrides film being prepared has good thermal stability and adhesive force.)

1. a kind of preparation method of the titanium oxynitrides film based on laser lift-off technique, which comprises the steps of:

Step 1, titanium nitride ceramic piece is placed on experiment porch, clean glass substrate is then placed into the titanium nitride On potsherd, keeps the lower surface of the glass substrate complete with the titanium nitride ceramic piece and fit closely；

Step 2, pulse laser is used to issue laser power as 2W, sweep speed is the laser of 400mm/s, by titanium nitride particles From the removing of titanium nitride ceramic on piece to the surface of the glass substrate and the titanium nitride particles are in conjunction with oxygen element, adhered to Titanium oxynitrides film layer below the glass substrate；

Step 3, use pulse laser issue laser power for 2W, sweep speed for 400mm/s or 700mm/s laser to institute It states titanium oxynitrides film layer to be irradiated, obtains the titanium oxynitrides film that nitrogen oxygen element content is changed.

2. the preparation method of the titanium oxynitrides film according to claim 1 based on laser lift-off technique, it is characterised in that:

Wherein, in the step 1, glass substrate is K9 glass substrate, diameter 30mm, with a thickness of 1.35mm.

3. the preparation method of the titanium oxynitrides film according to claim 1 based on laser lift-off technique, it is characterised in that:

Wherein, in the step 1, the diameter of titanium nitride ceramic piece is 50mm, with a thickness of 4mm.

4. the preparation method of the titanium oxynitrides film according to claim 1 based on laser lift-off technique, it is characterised in that:

Wherein, in the step 1, clean glass substrate obtains with the following method:

The ultrasonic cleaning for successively carrying out 15min respectively to the glass substrate with acetone, ethyl alcohol and deionized water, then uses nitrogen It is dry, obtain the glass substrate of clean dried.

5. the preparation method of the titanium oxynitrides film according to claim 1 based on laser lift-off technique, it is characterised in that:

Wherein, in the step 2 and the step 3, the wavelength for the laser that pulse laser issues is 1064nm, scan area It is 16mm*16mm.

6. prepared by a kind of preparation method using the titanium oxynitrides film described in Claims 1 to 5 based on laser lift-off technique Obtained titanium oxynitrides film.

Technical field

The invention belongs to technical field of film preparation, and in particular to a kind of titanium oxynitrides film and its be based on laser lift-off skill The preparation method of art.

Background technique

With the development of the mankind, the exhaustion of fossil fuel is more obvious using bring harm with it, and human society must not Think little of the influence of energy problem's generation.Solar energy catalysis is considered as the following ideal way for solving energy problem and environmental pollution One of diameter, and catalysis reaction is carried out using light, most important is exactly catalyst.

TiO₂The forbidden bandwidth of nano material is 3.2eV, there is strong absorption to ultraviolet light, be a kind of inexpensive clean without The catalyst of pollution and relative efficiency, can be used for photolysis water hydrogen and light degradation pollutant.But due to its forbidden bandwidth Larger, pure TiO₂Semiconductor material only just has photocatalytic activity under ultraviolet light.And it is radiated the tellurian sun It is ultraviolet light that light, which only has 5%, in order to make TiO₂Nano semiconductor material has catalytic effect under visible light, and researcher attempts A variety of methods, the metal cation doping of anion doped and Fe, Cr, Pt, Ta of N, F, S, B, C, P etc. etc., all TiO can be effectively reduced₂The forbidden bandwidth of nano semiconductor material, makes it have visible light catalysis activity.

Pass through N doping TiO₂Method preparation titanium oxynitrides nano thin-film catalyst have visible light catalytic characteristic, and And the efficiency of the visible light catalytic of the film catalyst is related with nitrogen element content.It is reported that researcher prepares titanium oxynitrides Nano thin-film and regulate and control the content of nitrogen oxygen element therein or need through complicated chemical method, or needs by accurate Equipment, technique is cumbersome, takes a long time, and certain pollution may be caused to environment.

Summary of the invention

The present invention is to carry out to solve the above-mentioned problems, and it is an object of the present invention to provide a kind of titanium oxynitrides film and its being based on The preparation method of laser lift-off technique.

The preparation method of the present invention provides a kind of titanium oxynitrides film based on laser lift-off technique has such spy Sign, includes the following steps: step 1, titanium nitride ceramic piece is placed on experiment porch, then places clean glass substrate To titanium nitride ceramic on piece, keeps the lower surface of glass substrate complete with titanium nitride ceramic piece and fit closely；Step 2, using arteries and veins Rushing laser and issuing laser power is 2W, and sweep speed is the laser of 400mm/s, by titanium nitride particles from titanium nitride ceramic on piece The surface of glass substrate and titanium nitride particles are removed in conjunction with oxygen element, obtains being attached to the titanium oxynitrides below glass substrate Film layer；Step 3, pulse laser is used to issue laser power as 2W, sweep speed is the laser pair of 400mm/s or 700mm/s Titanium oxynitrides film layer is irradiated, and the titanium oxynitrides film that nitrogen oxygen element content is changed is obtained.

In the preparation method of the titanium oxynitrides film provided by the invention based on laser lift-off technique, there can also be this The feature of sample: where in step 1, glass substrate is K9 glass substrate, diameter 30mm, with a thickness of 1.35mm.

In the preparation method of the titanium oxynitrides film provided by the invention based on laser lift-off technique, there can also be this The feature of sample: where in step 1, the diameter of titanium nitride ceramic piece is 50mm, with a thickness of 4mm.

In the preparation method of the titanium oxynitrides film provided by the invention based on laser lift-off technique, there can also be this The feature of sample: where in step 1, clean glass substrate obtains with the following method: with acetone, ethyl alcohol and deionized water according to The secondary ultrasonic cleaning for carrying out 15min respectively to glass substrate, it is then dry with nitrogen, obtain the glass substrate of clean dried.

In the preparation method of the titanium oxynitrides film provided by the invention based on laser lift-off technique, there can also be this The feature of sample: where in step 2 and step 3, the wavelength for the laser that pulse laser issues is 1064nm, and scan area is equal For 16mm*16mm.

A kind of nitrogen oxidation that the preparation method of the titanium oxynitrides film using above-mentioned based on laser lift-off technique is prepared Titanium film.

The action and effect of invention

The preparation method of titanium oxynitrides film based on laser lift-off technique involved according to the present invention, can pass through arteries and veins Impulse light obtains titanium oxynitrides film layer in the substrate of titanium nitride removing to removing substrate, when again using pulse laser pair It removes obtained titanium oxynitrides film layer to be irradiated, the content of nitrogen oxygen element can be regulated and controled, so that titanium oxynitrides film Constituent change.Therefore, the tune of the preparation method of the titanium oxynitrides film of the invention based on laser lift-off technique Control process is easy to operate, low in cost, additionally it is possible to apply in the preparation of Photocatalyzed Hydrogen Production catalyst, and be prepared using this method Obtained titanium oxynitrides film has good thermal stability and adhesive force, can apply organic in Photocatalyzed Hydrogen Production, light degradation Object etc..

Detailed description of the invention

Fig. 1 is the signal that pulse laser removing titanium nitride prepares titanium oxynitrides thin-film process in the embodiment of the present invention Figure；

Fig. 2 is that continuous wave laser irradiates titanium oxynitrides film to regulate and control its nitrogen oxygen element content in the embodiment of the present invention Schematic diagram；

Fig. 3 is that the constituent content diagram of sample obtained in the embodiment of the present invention one to embodiment three is intended to.

Specific embodiment

In order to which the technological means for realizing the present invention is easy to understand with effect, with reference to embodiments and attached drawing is to this Invention is specifically addressed.

The preparation method of titanium oxynitrides film based on laser lift-off technique of the invention, includes the following steps:

Step 1, titanium nitride ceramic piece is placed on experiment porch, clean glass substrate is then placed into sheet metal On, keep the lower surface of glass substrate complete with titanium nitride ceramic piece and fits closely.

Concrete operations are as follows: the ultrasound for successively carrying out 15min respectively to glass substrate with acetone, ethyl alcohol and deionized water is clear It washes, then dry with nitrogen, obtains the glass substrate of clean dried.First titanium nitride ceramic piece is placed on experiment porch, makes to nitrogenize Titanium potsherd is fitted closely with experiment porch, then the glass substrate of clean dried is placed on sheet metal, makes titanium nitride ceramic Piece is fitted closely with glass substrate.Wherein, the area of titanium nitride ceramic piece is greater than the area of glass substrate.

Step 2, pulse laser is used to issue laser power as 2W, sweep speed is the laser of 400mm/s, by titanium nitride Surface and titanium nitride particles of the particle from the removing of titanium nitride ceramic on piece to glass substrate obtain being attached to glass in conjunction with oxygen element Titanium oxynitrides film layer below glass substrate.

Concrete operations are as follows: removed with pulse laser, laser light glass substrate is by titanium nitride particles from titanium nitride It strips down on potsherd and is combined in the process with oxygen element and obtain titanium oxynitrides film, the titanium oxynitrides film is closely attached In the lower surface of K9 glass substrate.K9 glass substrate is taken down from titanium nitride ceramic on piece, the lower surface of K9 glass substrate is attached Have titanium oxynitrides film.

Step 3, pulse laser is used to issue laser power as 2W, sweep speed is the laser of 400mm/s or 700mm/s Titanium oxynitrides film layer is irradiated, titanium oxynitrides film is obtained.

Concrete operations are as follows: with pulse laser irradiation preparation titanium oxynitrides film, can to its nitrogen oxygen element content into The nitrogen oxygen element content of row regulation, the titanium oxynitrides film finally obtained has significant difference with before regulation.Wherein, scanning surface Product is 16mm*16mm.

The laser used in the present invention is Shanghai Fermi pulse laser FM-AW20, wavelength 1064nm.

Fig. 1 is the signal that pulse laser removing titanium nitride prepares titanium oxynitrides thin-film process in the embodiment of the present invention Figure.Wherein, Fig. 1 (a) is the schematic diagram before removing, and schematic diagram when Fig. 1 (b) is removing, Fig. 1 (c) is the schematic diagram after removing.

As shown in Figure 1, titanium nitride ceramic piece 2 is placed on 1 top of experimental bench, then glass substrate 3 is tightly attached to nitridation before removing The upper surface of titanium potsherd potsherd 2, when removing, the lower surface of laser irradiation to glass substrate 3 and titanium nitride ceramic piece 2 it is upper On surface, titanium nitride is removed onto 3 lower surface of glass substrate by pulse laser, forms titanium oxynitrides film 4.

Fig. 2 is that continuous wave laser irradiates titanium oxynitrides film to regulate and control its nitrogen oxygen element content in the embodiment of the present invention Schematic diagram.Wherein, Fig. 2 a is the schematic diagram of predose, and schematic diagram when Fig. 2 b is irradiation, Fig. 2 c is the schematic diagram after irradiation.

As shown in Fig. 2, predose, titanium oxynitrides film 4 is adhering closely in glass substrate 2, is placed on experimental bench 1 Side；When irradiation, in laser irradiation to titanium oxynitrides film 4；After irradiation, titanium oxynitrides film 5 by irradiation, still close patch It closes in glass substrate 2.By irradiation, the nitrogen oxygen element composition of titanium oxynitrides film layer is changed.