CN1684275A - Thin film material for sunlight blind area ultraviolet detector and its producing method - Google Patents

Thin film material for sunlight blind area ultraviolet detector and its producing method Download PDF

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CN1684275A
CN1684275A CN 200510049139 CN200510049139A CN1684275A CN 1684275 A CN1684275 A CN 1684275A CN 200510049139 CN200510049139 CN 200510049139 CN 200510049139 A CN200510049139 A CN 200510049139A CN 1684275 A CN1684275 A CN 1684275A
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film material
substrate
colloidal sol
acetate
thin
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CN100358159C (en
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季振国
何作鹏
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

A film material used in a solar blind zone UV detector characterizes that the formula of said film material is Nil-xMgxO and said material is manufactured by the following technology steps: 1, according to the atomic ratio of Mg/Ni in the formula, Mg acetate and Ni acetate in the formula, Mg acetate and Ni acetate in the weight ratio of 1:1.27-1:4.63 are put in a container to be mixed for 50-70minutes under 60deg.C taking hexanediol methyl oxide as the solvent, glacial acetic acid as the catalyst to get a uniform transparent green sol after 24 hours digestion. 2, coating a layer of sol on the substrate with the pulling method or spin coating method, 3, drying the substrate coated with the sol under 80deg.C, heat-processing it for 1-2h under 500deg.C, then processing it under 900-1100deg.C, for 2-6h and cooling it naturally to get the necessary film material.

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 (GaAlN) 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 λ = 1240 E g = 248 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 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.
CNB2005100491396A 2005-02-28 2005-02-28 Thin film material for sunlight blind area ultraviolet detector and its producing method Expired - Fee Related CN100358159C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101621066B (en) * 2008-07-02 2011-06-01 中国科学院半导体研究所 GaN-based solar-blind UV detector area array and manufacturing method thereof
CN103337590A (en) * 2013-05-30 2013-10-02 浙江大学 Highly responsive organic solar blind type ultraviolet detector

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US9928727B2 (en) 2015-07-28 2018-03-27 Carrier Corporation Flame detectors
US10126165B2 (en) 2015-07-28 2018-11-13 Carrier Corporation Radiation sensors
US9806125B2 (en) 2015-07-28 2017-10-31 Carrier Corporation Compositionally graded photodetectors
US9865766B2 (en) 2015-07-28 2018-01-09 Carrier Corporation Ultraviolet photodetectors and methods of making ultraviolet photodetectors

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002080823A (en) * 2000-09-08 2002-03-22 Kinya Adachi Ultraviolet ray insulating agent
JP4188672B2 (en) * 2002-05-31 2008-11-26 篠田プラズマ株式会社 Photochromic body, photochromic material and method for producing the same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101621066B (en) * 2008-07-02 2011-06-01 中国科学院半导体研究所 GaN-based solar-blind UV detector area array and manufacturing method thereof
CN103337590A (en) * 2013-05-30 2013-10-02 浙江大学 Highly responsive organic solar blind type ultraviolet detector
CN103337590B (en) * 2013-05-30 2015-12-09 浙江大学 High-responsivity organic solar blind type ultraviolet detector

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