CN100358159C - Thin film material for sunlight blind area ultraviolet detector and its producing method - Google Patents

Abstract

The present invention relates to a thin film material for a sunlight blind area ultraviolet detector, which is characterized in that the formula of the thin film material is Ni <1-X> Mg XO, wherein X is between 0.2 and 0.3. The fabrication technology of the materials has the following processing steps: 1. according to the atomic ratio of magnesium/nickel in the formula of Ni<1-X> Mg XO, magnesium acetate and magnesium acetate in the weight ratio of 1: 1.27 to 1: 4.63 are put into a container to be mixed for 50 to 70 minutes at 60 DEG C. by using glycol methyl ether as the solvent and glacial acetic acid as the catalyst; uniform transparent green the colloidal sol is obtained after placement and ageing for 24 hours; 2. a layer of colloidal sol is coated on a substrate by using a pulling method or a spin-coating method; 3. the substrate coated with the colloidal sol is dried under 80 DEG C. and is processed for one to two hours under 500 DEG C. in a heating mode, and then, the substrate coated with the colloidal sol is cooled naturally after heat treatment for 2 to 6 hours under the temperature of 900 to 1100 DEG C. to obtain the thin film material. Compared with the prior art, the present invention has the prominent advantages that the thin film material has simple manufacturing process, nontoxicity and low cost; the thin film material is an ideal thin film material used for the sunlight blind area ultraviolet detector.

Description

Thin-film material and manufacture method thereof that a kind of day blind region ultraviolet detector device used

Technical field

The present invention relates to a kind of thin-film material, particularly thin-film material and the manufacture method thereof used of a kind of day blind region ultraviolet detector device.

Background technology

Along with the development of spectral technique, the people's attention focus shifts to the short wavelength gradually, and wherein, the spectrum that wavelength is in 240～280nm scope is a special region.Because atmosphere is to the absorption of sunlight, the light in 240～280nm scope is absorbed and can't arrives earth surface, do not have the light in this wave band near the sunlight the earth surface, so this wave band is called as a day blind area.Because day blind region ultraviolet detector device is insensitive to sunlight, can be under the situation that not influenced by sunlight, survey the wake flame that aircraft from the enemy, guided missile etc. send, also can be used for fire alarm, the aspects such as online detection of ultraviolet communication, high-tension line.

At present, the thin-film material that day blind region ultraviolet detector device is used mainly is aluminum gallium nitride (GaAIN) system, this material require adopts film preparing technologies such as metal organic chemical vapor deposition, molecular beam epitaxy, exist raw material and equipment very expensive, complex manufacturing technology, the cost height, defective such as organic source toxicity is big.

Summary of the invention

The purpose of this invention is to provide thin-film material and manufacture method thereof that a kind of day blind region ultraviolet detector device used, the optical energy gap of the thin-film material of making is 5eV, corresponding ABSORPTION EDGE wavelength is 245～255nm, this thin-film material is very little to the response of sunlight, and it is sensitive especially to the response of the ultraviolet light of same optical power density, this thin-film material manufacturing process is simple, avirulence, and cost is low.

The thin-film material that a kind of day blind region ultraviolet detector device used, it is characterized in that: this thin-film material is the nickel magnesium oxide, its molecular formula is Ni _1-XMg _XO, 0.2≤X in the formula≤0.3.

A kind of method of making above-mentioned material is characterized in that adopting following process steps:

A) according to molecular formula Ni _1-XMg _XThe scope of O and X is 0.2～0.3, the scope of corresponding magnesium/nickle atom ratio is 1: 4～1: 2.33, the magnesium acetate of corresponding above-mentioned atomic ratio and the weight ratio of nickel acetate are 1: 2.7～1: 4.63, raw acetic acid nickel and magnesium acetate are put into container by required proportioning, hexylene glycol methyl ether with 1 unit volume is a solvent, is catalyst with the glacial acetic acid of 0.05～0.1 unit volume, stirs 50～70 minutes down at 60 ℃, place ageing 24 hours, obtain the green colloidal sol of homogeneous transparent;

B) clean substrate is immersed in the colloidal sol, on substrate, be coated with last layer colloidal sol, perhaps adopt spin-coating method on substrate, to be coated with last layer colloidal sol with czochralski method;

C) the substrate that scribbles colloidal sol 80 ℃ of down oven dry 30～40 minutes, 500 ℃ of following heat treatments 1～2 hour, at 900～1100 ℃ of following high-temperature heat treatment natural cooling after 2～6 hours, obtain required thin-film material again.

There is a kind of in the silicon chip of thick oxygen silicon on substrate adopting quartz glass, sapphire and surface, and the chemical formula of nickel acetate is Ni (Ac) ₂4H ₂O, the chemical formula of magnesium acetate are Mg (Ac) ₂4H ₂O.

With prior art relatively, outstanding advantage of the present invention is: this thin-film material manufacturing process is simple especially, avirulence, and cost is low, is ideal a kind of in the thin-film material that uses of day blind region ultraviolet detector device.

Description of drawings

Fig. 1 is to through 2 hours nickel magnesium oxide Ni of 1000 ℃ of following heat treatments _0.7Mg _0.3The energy gap test result of O film, ordinate wherein are absorption coefficient and photon energy long-pending square, and abscissa is eV.As seen its energy gap is 5eV, and corresponding ABSORPTION EDGE wavelength is $\mathrm{\&lambda;}=\frac{1240}{E_g}=248\mathrm{nm}$ , be positioned at solar blind

Fig. 2 is nickel magnesium oxide film Ni _0.8Mg _0.2O is to the photoconductive response curve of sunlight A and 254nm ultraviolet light B, and abscissa is time (second), and ordinate is normalization photoconduction (arbitrary unit).As seen this film is very little to the response of sunlight, and the ultraviolet light of same optical power density is had very high response.

Embodiment

Embodiment 1:

The thin-film material that a kind of day blind region ultraviolet detector device used, its molecular formula is Ni _0.7Mg _0.3O, i.e. x=0.3.Adopt following process steps: A) according to molecular formula Ni _0.7Mg _0.3Magnesium among the O/nickle atom ratio is put into glass container with 2g magnesium acetate and 5.5g nickel acetate, adds the chemical pure hexylene glycol methyl ether of 100ml then, add the chemical pure glacial acetic acid of 5ml again, stirred 70 minutes down at 60 ℃, place ageing 24 hours, obtain the green colloidal sol of homogeneous transparent; B) adopt spin-coating method on substrate, to be coated with last layer colloidal sol; C) the substrate that scribbles colloidal sol 80 ℃ of down oven dry 40 minutes, 500 ℃ of following heat treatments 2 hours, at 900 ℃ of following high-temperature heat treatment natural cooling after 6 hours, obtain required thin-film material again.When adopting spin-coating method to be coated with last layer colloidal sol on substrate, its rotary speed is 3000rpm, and substrate is a quartz glass plate.The energy gap of this thin-film material is shown in Fig. 1.

Embodiment 2:

The thin-film material that a kind of day blind region ultraviolet detector device used, its molecular formula is Ni _0.8Mg _0.2O, promptly x=0.2 adopts following process steps: A) according to molecular formula Ni _0.8Mg _0.2Magnesium among the O/nickle atom ratio is put into glassware with 1g magnesium acetate and 4.63g nickel acetate, adds the chemical pure hexylene glycol methyl ether of 100ml then, and the chemical pure glacial acetic acid of 10ml, stirred 50 minutes down at 60 ℃, place ageing 24 hours, obtain the green colloidal sol of homogeneous transparent; B) clean substrate is immersed in the colloidal sol, on substrate, be coated with last layer colloidal sol with czochralski method; C) the substrate that scribbles colloidal sol 80 ℃ of down oven dry 30 minutes, 500 ℃ of following heat treatments 1 hour, at 1100 ℃ of following high-temperature heat treatment natural cooling after 2 hours, obtain required thin-film material again.When adopting czochralski method to be coated with last layer colloidal sol on substrate, its pull rate is that per minute lifts 10 centimetres, and substrate is a sapphire sheet.The photoconductive response curve to sunlight A and 254nm ultraviolet light B of this thin-film material is shown in Fig. 2.

Claims (2)

1. One kind day the thin-film material used of blind region ultraviolet detector device, it is characterized in that: this thin-film material is the nickel magnesium oxide, its molecular formula is Ni _1-XMg _XO, 0.2≤X in the formula≤0.3.
2. 2. method of making the described material of claim 1 is characterized in that adopting following process steps:

   A) according to molecular formula Ni _1-XMg _XThe scope of O and X is 0.2～0.3, the scope of corresponding magnesium/nickle atom ratio is 1: 4～1: 2.33, the magnesium acetate of corresponding above-mentioned atomic ratio and the weight ratio of nickel acetate are 1: 2.7～1: 4.63, raw acetic acid nickel and magnesium acetate are put into container in required ratio, hexylene glycol methyl ether with 1 unit volume is a solvent, and the glacial acetic acid of 0.05～0.1 unit volume is a catalyst, stirs 50～70 minutes under 60 ℃ of situations, place ageing 24 hours, obtain the green colloidal sol of homogeneous transparent;

   B) clean substrate is immersed in the colloidal sol, on substrate, be coated with last layer colloidal sol, perhaps adopt spin-coating method on substrate, to be coated with last layer colloidal sol with czochralski method;

   C) substrate that scribbles colloidal sol was dried 30～40 minutes under 80 ℃ of situations, heat treatment is 1～2 hour under 500 ℃ of situations, and high-temperature heat treatment natural cooling after 2～6 hours under 900～1100 ℃ of situations obtains required thin-film material again.

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