KR19980027003A - Invisible light emitting material and manufacturing method - Google Patents

Invisible light emitting material and manufacturing method Download PDF

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KR19980027003A
KR19980027003A KR1019960045650A KR19960045650A KR19980027003A KR 19980027003 A KR19980027003 A KR 19980027003A KR 1019960045650 A KR1019960045650 A KR 1019960045650A KR 19960045650 A KR19960045650 A KR 19960045650A KR 19980027003 A KR19980027003 A KR 19980027003A
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compound
hours
light emitting
emitting material
matrix
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KR0178356B1 (en
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신길승
안승덕
김홍조
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민태형
한국조폐공사
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7776Vanadates; Chromates; Molybdates; Tungstates

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Abstract

본 발명은, 이트륨(Yttrium) 화합물, 실리콘(Silcon) 화합물 및 바나듐(Vanadium) 화합물의 산화물을 매트릭스로 하고, 이에 활성화제로서 Nd2O3과 Er2O3을 첨가하여 균일 혼합하고, 1단계 반응으로 산화성 분위기에서 600-700℃로 3-5시간 소성시킨후 직경이 5-15μm 정도가 되게 분쇄하며, 2단계 반응으로 이 분쇄물을 1000-1200℃로 3-5시간 소정시킨후 직경 2-4μm 정도의 크기로 분쇄하고, 3단계 반응으로 2단계 반응물을 500-700℃에서 1-3시간 정도 소성하고 약 1μm정도로 분쇄하여 제조하는, 분자식이 Y2SiV2O10:Nd+3, Er+3인 비가시 발광물질과 그 제조방법을 제공하기 위한 것으로, UV광 및 가시광을 조사할 경우 적외선광을 발광케하므로서, 특히, 은행권 및 유가증권류등 특수 인쇄물에 10mm2정도 면적으로 본 발명물질을 포함하는 잉크를 인쇄하므로서 위조방지 효과를 얻을 수 있게 하며, 은행권등의 기계적 자동처리를 위한 기계인식 기능을 부여할 수 있게 하고 천연색 복사기에 의한 복사를 방지할 수 있게 하는 효과를 나타낼 수 있게 하는 것임.In the present invention, an oxide of a yttrium compound, a silicon compound, and a vanadium compound is used as a matrix, and Nd 2 O 3 and Er 2 O 3 are added to the matrix as an activator, and uniformly mixed. After calcination at 600-700 ° C. for 3-5 hours in an oxidizing atmosphere, the powder is pulverized to a diameter of 5-15 μm, and the pulverized product is prescribed for 3-5 hours at 1000-1200 ° C. in a two-stage reaction. A molecular formula of Y 2 SiV 2 O 10 : Nd +3 , which is prepared by pulverizing to a size of about -4 μm, sintering the second stage reactant at 500-700 ° C. for 1-3 hours and pulverizing to about 1 μm in a three-step reaction. Er +3 invisible light emitting material and a method of manufacturing the same, and when irradiated with UV light and visible light emits infrared light, especially in banknotes and securities, such as special printed materials such as 10mm 2 area Anti-counterfeiting effect by printing ink containing invention material It is possible to obtain an effect, to give a mechanical recognition function for automatic mechanical processing of banknotes, etc., and to have an effect of preventing copying by a color copier.

Description

비가시 발광물질(非可視 發光物質) 및 그 제조방법Invisible light emitting material and its manufacturing method

본 발명은 UV광(紫外光線:Ultra-Violet) 및 가시광(Visible광:可視光)을 조사할 경우 IR광(赤外光線:Infrared)을 발광(發光:Emission)하는 비가시 발광물질(非可視 發光物質)과 그 제조 방법에 관한 것으로 특히, 은행권 및 유가증권류등 특수 인쇄물에 10mm2정도 면적으로 본 발명물질을 포함하는 잉크를 인쇄하므로서 위조방지 효과를 얻을 수 있게 하며, 은행권등의 기계적 자동처리를 위한 기계인식 기능을 부여할 수 있게 하고 천연색 복사기에 의한 복사를 방지할 수 있게 하는 효과를 나타낼 수 있는 비가시 발광물질과 그 제조방법을 제공하기 위한 것이다.The present invention is an invisible light emitting material that emits infrared light when irradiated with UV light (Ultra-Violet) and visible light (Visible light).發光 物質) and the manufacturing method thereof, in particular, by printing ink containing the present invention in the area of about 10mm 2 on special printed materials, such as banknotes and securities, it is possible to obtain the anti-counterfeiting effect, and mechanical automatic such as banknotes It is to provide an invisible light-emitting material and a method of manufacturing the same, which can give a mechanical recognition function for treatment and can exhibit an effect of preventing radiation by a color copier.

일반인쇄의 한 분야중에 인쇄시 잉크(Ink)의 건조속도를 빠르게 하기 위해 이용되는 자외선 경화잉크(紫外線 硬化 잉크:UV Curing Ink)와 적외선 경화잉크(赤外線 硬化잉크:IR Curing Ink)가 있다. 자외선 경화잉크는 감광성 수지, 감광성 모노머, 광개시제(光開始劑)를 주성분으로 한 전색제(Vehicle)를 사용한 잉크로 자외선(紫外線)을 조사(照射)하여 잉크를 순간적으로 건조시키는 잉크이며, 적외선 경화잉크는 IR Varnish, Gel Varnish, Solvent를 주성분으로 한 전색제를 사용함으로써 잉크의 건조속도를 빠르게 하기 위한 잉크의 종류를 말하는 것으로 본 발명과는 전혀 다른 분야로서 용어상의 혼동이 없어야 할 것이다.One of the fields of general printing is UV Curing Ink and IR Curing Ink which are used to speed up the drying speed of Ink. UV curable ink is ink using a photosensitive resin, a photosensitive monomer, and a vehicle containing a photoinitiator as a main component, which irradiates ultraviolet rays to dry the ink instantly, and an infrared curable ink Refers to a kind of ink for increasing the drying speed of the ink by using a colorant mainly composed of IR Varnish, Gel Varnish, and Solvent. There should be no confusion in terms as a field completely different from the present invention.

현재 국내외 은행권이나 수표 등에 위조방지를 위하여 인쇄되어 자외선광에 의해 형광이 발해지는 형광물질(螢光物質)은 산업기술의 전반적 진전에 따라 누구나 조그만 관심을 두면 비교적 쉽게 구할 수 있는 UV 램프로서 은행권등에 인쇄된 형광을 비교적 쉽게 확인할 수 있으며, 자성(磁性)잉크 또한 일반 인쇄물에 보편적으로 이용되는 추세로서 위조등에 이를 도용할 여지가 많다 할 수 있겠다.Currently, fluorescent materials printed by domestic and foreign banknotes and checks to prevent falsification are emitted by ultraviolet light, and UV lamps are relatively easy to obtain if anyone pays little attention to the general progress of industrial technology. Printed fluorescence can be identified relatively easily, and magnetic ink is also widely used in general printed matters, and there is a lot of room for theft.

그러므로 은행권, 유가증권류 및 기타 보안문서 등 특수 인쇄물의 위조방지를 위해, 발광(發光)상태가 눈에 보이지 않는 적외선광을 발광하는 발광물질인 비가시 발광물질을 은행권이나 유가증권류 등 특수 인쇄물에 10mm2이내의 작은 면적으로 인쇄할 경우 위조방지는 물론 진위감별(眞僞鑑別), 손권분류(損券分類), 자동계수(自動計數), 환전(換錢)등 기계적 자동처리 기능인 자동정사 기능(自動整査 機能)의 극대화와 천연색 복사방지를 기할 수 있을 것으로 기대된다.Therefore, in order to prevent counterfeits of special printed materials such as banknotes, securities, and other security documents, invisible light emitting materials that emit infrared light with invisible light can be printed on special printed materials such as banknotes or securities. When printing on a small area of less than 10mm 2 , the automatic inspection function is a mechanical automatic processing function such as anti-counterfeiting, authenticity discrimination, hand classification, automatic counting and currency exchange. It is expected to be able to maximize the color and prevent the color copying.

발광물질이 발광하게 되는 것은, 어떤 원소(元素)가 전자궤도(電子軌道:Orbital)에 전자가 부족한 상태 즉, Energy의 최저 상태인 기저상태(基底狀態:Ground State)에 있는 경우, 이에 에너지를 공급하게 되면 기저상태의 물질이 에너지를 흡수하여 여기상태(勵起狀態:Excited State)로 되고, 당해 물질로부터 외부 에너지를 제거했을때 전자가 여기상태에서 기저상태로 떨어지면서 에너지를 방출하며 발광하게 하는 전자적 과정(電子的 過程)때문이다.The light emitting material emits light when an element is in a state in which an electron orbit is deficient in an electron orbit, that is, in a ground state which is the lowest state of energy. When supplied, the substance in the ground state absorbs energy into an excited state, and when the external energy is removed from the substance, electrons fall from the excited state to the ground state to emit energy and emit light. It is because of the electronic process.

한편 희토류원소(稀土類 元素)들의 이온(Ion)이 나타내는 광스펙트럼(光 Spectrum)은 예민한 Peak를 나타내는 특징이 있으며, 이것은 흡수 Spectrum과 같은 모양으로 4f 전자천이(電子遷移)와 관련되는 것으로서 발광파장은 모체결정(母體결정結晶)에 강하게 의존하며 4f내 천이(遷移)에서 발광은 이온(Ion)의 종류에 따라 파장의 Spectrum 폭이 좁은 발광을 나타낸다.On the other hand, the optical spectrum represented by the ions of rare earth elements is characterized by a sharp peak, which is shaped like an absorption spectrum and is associated with 4f electron transitions and emits light. Is strongly dependent on the parent crystal, and the light emission in the transition within 4f shows light emission with a narrow spectrum width depending on the type of ion.

본 발명은 위와 같은 발광원리 및 희토류 원소의 특성을 이용하여 본 발명의 빗가시 발광물질을 제공할 수 있게 한 것이다. 즉, 본 발명의 비가시 발광물질은 800-1500nm의 발광영역을 가지는 네오디뮴(Neodymium:Nd)과 700-1500nm의 발광영역을 가지는 어븀(Erbium:Er)을 발광물체의 활성화제로 하고 Y2SiV2O10을 매트릭스(Matrix)로 하여 제조하므로서, 자외선 및 가시광선 영역인 280-630nm의 파장 범위의 광에 의하여 여기되어 비가시 적외선 영역인 800-1500nm의 발광주 파장(Emission peak wave length)을 갖게 하여 발광상태를 육안으로는 확인할 수 없고, Mercury Lamp, He-Ne, Laser Monochromator, Scanning controller등 각종 광학장치를 이용하여야만 발광특성을 확인할 수 있게 한 것이며, 이러한 특성을 은행권이나 유가증권 등 특수인쇄물에 사용하기 위해 특별히 개발한 물질이다.The present invention is to provide a non-visible light emitting material of the present invention by using the above-described light emission principle and characteristics of the rare earth element. That is, the invisible light emitting material of the present invention is made of neodymium (Neodymium (Nd)) having an emission region of 800-1500nm and Erbium (Erbium: Er) having an emission region of 700-1500nm as the activator of the light emitting material Y 2 SiV 2 By manufacturing O 10 as a matrix, it is excited by light in the wavelength range of 280-630 nm, which is an ultraviolet and visible light region, to have an emission peak wave length of 800-1500 nm, which is an invisible infrared region. It is impossible to check the emission state with the naked eye, and it is possible to check the emission characteristics only by using various optical devices such as Mercury Lamp, He-Ne, Laser Monochromator, Scanning controller, etc. It is a material specifically developed for use.

이와 같이 비가시 영역(非可視 領域) 파장의 빛을 발하는 특성을 갖는 본 발명의 비가시 발광물질은 활성화제(Activator)로 네오디뮴과 어븀을 사용하고 매트릭스로 Y2SIV2O10을 사용하여 Y2SiV2O10:Nd+3, Er+3의 구조를 가지게 한 것으로 그 제조방법을 설명하면 다음과 같다.Thus, the invisible light emitting material of the present invention having the characteristic of emitting light in the invisible region wavelength uses neodymium and erbium as an activator and Y 2 SIV 2 O 10 as a matrix. It has a structure of 2 SiV 2 O 10 : Nd + 3 , Er + 3 and the manufacturing method is as follows.

*편의상 Y2SiV2O10:Nd+3, Er+3의 명칭을 IVM-1이라고 한다.For convenience, the names of Y 2 SiV 2 O 10 : Nd +3 and Er +3 are called IVM-1.

본 발명은 이트륨(Yttrium)화합물[Y2(CO3)3, Y(NO3)3, Y2O3, Y2(C2O4)3, YCl3], 실리콘(Silcon) 화합물[SiO2, Na2SiO3] 및 바나듐(Vanadium) 화합물[VCl3, V2O5, NH4VO3]의 산화물을 매트릭스로 하고, 이에 활성화제로서 네오디뮴 화합물과 어븀 화합물을 혼합하는 바, 네오디뮴 화합물은 Nd2O3인 것이 바람직하며, 그 량은 0.001mol인 것이 바람직하고, 어븀 화합물 Er2O3인 것이 바람직하고 그 량은 0.0003mol인 것이 바람직하다. 위와같이 이트륨화합물과 실리콘 화합물 및 바나듐 화합물의 산화물을 매트릭스로 하고 이에 네오디뮴화합물과 어븀화합물을 활성화제로 혼합한 후, 균일하게 혼합하고, 1단계 반응으로 산화성 분위기에서 600-700℃로 3-5시간 소성시킨후 직경이 5-15μm정도가 되게 분쇄하며, 2단계 반응으로 이 분쇄물을 1000-1200℃로 3-5시간 소성시킨후 직경 2-4μm 정도의 크기로 분쇄하고, 3단계 반응으로 2단계 반응물을 500-700℃에서 1-3시간 정도 소성하고 약 1μm정도로 분쇄하여 본 발명의 물질인 Y2SiV2O10:Nd+3, Er+3의(ⅣM-1)을 제조한다.The present invention is a yttrium compound [Y 2 (CO 3 ) 3 , Y (NO 3 ) 3 , Y 2 O 3 , Y 2 (C 2 O 4 ) 3 , YCl 3 ], a silicon compound [SiO 2 , Na 2 SiO 3 ] and a vanadium compound [VCl 3 , V 2 O 5 , NH 4 VO 3 ] oxide as a matrix, and a neodymium compound and an erbium compound are mixed as an activator The silver is preferably Nd 2 O 3 , the amount thereof is preferably 0.001 mol, the erbium compound Er 2 O 3 is preferred, and the amount thereof is preferably 0.0003 mol. As above, oxides of yttrium compound, silicon compound and vanadium compound are used as a matrix, and neodymium compound and erbium compound are mixed as an activator, and then uniformly mixed and mixed at 600-700 ° C. in an oxidizing atmosphere for 3-5 hours in a one-step reaction. After firing, the powder is pulverized to a diameter of about 5-15 μm, and the pulverized product is calcined at 1000-1200 ° C. for 3-5 hours in a two-step reaction, and then pulverized to a size of about 2-4 μm in diameter, Step The reactant was calcined at 500-700 ° C. for 1-3 hours and ground to about 1 μm to prepare (IVM-1) of Y 2 SiV 2 O 10 : Nd +3 and Er +3 as materials of the present invention.

상기의 제조 방법에 있어서, 산화물인 매트릭스는 상품화되어 공지된 바 있는 Y2SiV2O10인 것이 바람직하며, 활성화제는 Nd의 함량이 매트릭스량의 0.2-0.3%되게 Nd 화합물[NdCl3, NdF3, (CH3CO2)Nd, Nd(NO3)3, Nd2O3, Nd2(SO4)3]과, Er 함량이 매트릭스량의 0.1%되게 Er 화합물[ErCl3, Er(CO3)3, ErF3, Er(NO3)3, Er2O3]을 첨가하는 것이 바람직하다.In the above production method, the matrix, which is an oxide, is preferably Y 2 SiV 2 O 10 which has been commercialized and known, and the activator is an Nd compound [NdCl 3 , NdF so that the Nd content is 0.2-0.3% of the matrix amount. 3 , (CH 3 CO 2 ) Nd, Nd (NO 3 ) 3 , Nd 2 O 3 , Nd 2 (SO 4 ) 3 ] and the Er compound [ErCl 3 , Er (CO) so that the Er content is 0.1% of the matrix amount. 3 ) 3 , ErF 3 , Er (NO 3 ) 3 , Er 2 O 3 ] is preferred.

이와 같은 본 발명의 비가시 발광물질의 제조방법을 실시예에 따라 상세히 설명하면 다음과 같다.Such a method of manufacturing the invisible light emitting material of the present invention will be described in detail with reference to Examples.

[실시예]EXAMPLE

제1공정1st process

원료 조성비는 표 1과 같이 하여 볼밀(Ball Mill)에서 충분히 균일 혼합하여 혼합물 A를 제조한다.The raw material composition ratio is sufficiently uniformly mixed in a ball mill as shown in Table 1 to prepare a mixture A.

[표 1] 원료조성비[Table 1] Raw Material Composition Ratio

제2공정2nd process

혼합물 A를 Alumina Crucible에 장입하여 산화성 분위기중의 전기로에서 650℃로 4시간 가열 한후 직경 10μm정도의 크기로 분쇄하여 반응물 B를 얻는다.Charge A mixture into Alumina Crucible, heat it to 650 ° C. for 4 hours in an electric furnace in an oxidizing atmosphere, and grind to a size of about 10 μm in diameter to obtain reactant B.

제3공정3rd process

반응물 B를 역시 산화성 분위기중의 전기로에서 1100℃로 4시간 가열한 후 직경 3μm 정도로 분쇄하여 반응물 C를 얻는다.Reactant B is also heated to 1100 ° C. for 4 hours in an electric furnace in an oxidizing atmosphere and then ground to a diameter of 3 μm to obtain reactant C.

제4공정4th process

반응물 C를 산화성 분위기중의 전기로에서 600℃로 2시간 가열한 후 직경 1μm정도로 미분쇄하므로써 반응을 종결하여 본 발명의 비가시 발광물질을 얻는다.The reaction C is terminated by heating the reactant C at 600 ° C. for 2 hours in an oxidizing atmosphere and finely pulverizing it to about 1 μm in diameter to obtain the invisible light emitting material of the present invention.

이상과 같은 단계별 반응을 종결하여 얻은, 본 발명의 물질인 ⅣM-1을 실제 인쇄물에 인쇄할 경우에 있어서의 인쇄효과 및 발광강도를 검토하기 위해, Alkyd Resin 및 Rosin Modified Phenolic Resin을 주성분으로 하는 평판잉크 Varnish[대한잉크(주) 제품]를 전색제로 사용하여 잉크 제조 적성을 검토하고 광특성 변화 요인 등의 실험을 실시한 결과 아래와 같이 실험결과를 얻을 수 있었다.In order to examine the printing effect and luminous intensity in the case of printing IVM-1, the material of the present invention, on the actual printed matter obtained by terminating the above-described stepwise reaction, a flat plate mainly composed of Alkyd Resin and Rosin Modified Phenolic Resin. Using ink varnish (manufactured by Daehan Ink Co., Ltd.) as a colorant, the aptitude of ink production was examined and experiments such as optical characteristic change factors were obtained.

실험 1:Experiment 1:

투입율과 발광강도Input rate and luminous intensity

ⅣM-1의 투입율이 10,20,30,40Wt%인 잉크를 제조하여 동일 인쇄 Pattern을 갖는 인쇄물로 인쇄(잉크층 두께:15μm)하여 발광강도를 측정한 결과 다음의 표 2와 같이 투입율에 비례하는 발광강도(Emission Intensity)를 얻을 수 있었다.As a result of measuring the luminous intensity by preparing the ink having the input rate of ⅣM-1 of 10,20,30,40Wt% and printing it with printed materials having the same printing pattern (ink layer thickness: 15μm), Emission intensity in proportion to was obtained.

[표 2] 투입율과 발광강도[Table 2] Input rate and emission intensity

실험2Experiment 2

잉크층 두께와 발광강도Ink layer thickness and luminous intensity

ⅣM-1 투입량이 20Wt%인 잉크로 3,5,10,20,30,40μm 잉크층 두께를 갖는 인쇄물을 제작하여 발광강도를 측정한 결과 다음의 표 3과 같이 잉크층 두께에 비례하는 발광강도를 얻을 수 있었다.As a result of measuring the luminous intensity of a printed matter having a 3,5,10,20,30,40μm ink layer thickness using an ink having IVM-1 input amount of 20 Wt%, the luminous intensity was proportional to the thickness of the ink layer as shown in Table 3 below. Could get

[표 2] 잉크층 두께별 발광강도[Table 2] Luminous intensity by ink layer thickness

실험 3:Experiment 3:

유색안료의 영향성 검토Review of the impact of colored pigments

인쇄물 제조시 유색안료들의 과간섭 영향을 검토하기 위해 ⅣM-1을 20%로 고정하고 유색안료[무색계(無色系), Red, Yellow계, Green계, Blue계, Black계]의 투입율을 8%, 잉크층 두께는 15μm로 하여 발광강도를 측정한 결과, 무색RedYellowGreenBlueBlack순으로 강도가 약화됨을 알았다.In order to examine the effects of over-pigmentation of colored pigments in the production of printed materials, fix IVM-1 to 20% and adjust the input rate of color pigments (colorless, red, yellow, green, blue, and black). %, The thickness of the ink layer was measured to be 15μm, the emission intensity was measured, it was found that the strength is weakened in the order of colorless RedYellow Green Blue Black.

이 실험에서 사용된 색상별 유색안료 명칭은 다음과 같다.The color pigments by color used in this experiment are as follows.

1) 무색계(Ca계 체질 안료)1) Colorless system (Ca constituent pigment)

2) Red계(Symuler Fast Red)2) Red system (Symuler Fast Red)

3) Yellow계(Symulcr Fast Yellow)3) Yellow system (Symulcr Fast Yellow)

4) Green계(Symuler Fast Yellow{4}+Phthalocyanine Blue{1})4) Green (Symuler Fast Yellow {4} + Phthalocyanine Blue {1})

5) Blue계(Phthalocyanine Blue)5) Blue system (Phthalocyanine Blue)

6) Black계(Carbon Black)6) Black (Carbon Black)

실험 4:Experiment 4:

평판 인쇄 실험Flatbed printing experiment

평판 인쇄 적성 검토 및 인쇄물의 다량 제조를 위해, 본 발명의 물질인 ⅣM-1을 혼합하여 평판잉크를 제조하되, 그 물성이 Tack(60Sec, 32℃ 100m/min) 148, Flow(30Sec, 25℃) 807dyne/cm2이 되게 제조하여, 데라루 지오리사(De La Rue Giori社:스위스)의 평판 인쇄기 상에서 평판인쇄 실험을 실시한 전이성 등 제반 인쇄적성과 내약품성, 내광성 등 제반내성과 발광효과등 특수인쇄물로서의 효과가 양호하였다. 이 실험을 위하여 제조된 잉크의 조성비는 다음과 같았다.In order to examine aptitude printing and manufacture a large quantity of printed matter, IVM-1, which is a material of the present invention, is mixed to prepare a flat ink, and the physical properties thereof are Tack (60Sec, 32 ℃ 100m / min) 148, Flow (30Sec, 25 ℃ Manufactured to be 807 dyne / cm 2 and carried out plate printing experiments on De La Rue Giori (Switzerland) flatbed printing machine, including general printing aptitude, chemical resistance, light resistance, etc. The effect as a printed matter was favorable. The composition ratio of the ink prepared for this experiment was as follows.

평판 잉크 조성비Wt%Flat Ink Composition Wt%

ⅣM-1 17.4ⅣM-1 17.4

Symuler Fast Red 1.1Symuler Fast Red 1.1

평판 Varnish 71.0Reputation Varnish 71.0

Wax 4.5Wax 4.5

용제 5.8Solvent 5.8

건조제 0.2Desiccant 0.2

100100

*용제는 비점 290℃인 석유계 용제임* Solvent is petroleum solvent with boiling point 290 ℃

Claims (6)

분자식이 Y2SiV2O10:Nd+3, Er+3인 비가시 발광물질.An invisible light emitting material having a molecular formula of Y 2 SiV 2 O 10 : Nd +3 , Er +3 . 이트륨(Yttrium)화합물[Y2(CO3)3, Y(NO3)3, Y2O3, Y2(C2O4)3, YCl3], 실리콘(Silcon)화합물[SiO2, Na2SiO3] 및 바나듐(Vanadium)화합물[VCl3, V2O5, NH4VO3]의 산화물을 매트리스로 하고, 이에 활성화제로서 네오디뮴(Nd) 화합물과 어븀(Er) 화합물을 혼합하고, 1단계 반응으로 산화성 분위기에서 600-700℃로 3-5시간 소성시간 후 직경이 5-15μm정도가 되게 분쇄하며, 2단계 반응으로 이 분쇄물을 1000-12000℃로 3-5시간 소성시킨후 직경 2-4μm 정도의 크기로 분쇄하고, 3단계 반응으로 2단계 반응물을 500-700℃에서 1-3시간 정도 소성하고 약 1μm정도로 분쇄하여 제조하는 것을 특징으로 하는 비가시 발광 물질의 제조방법.Yttrium Compound [Y 2 (CO 3 ) 3 , Y (NO 3 ) 3 , Y 2 O 3 , Y 2 (C 2 O 4 ) 3 , YCl 3 ], Silicon Compound [SiO 2 , Na Oxide of 2 SiO 3 ] and vanadium compound [VCl 3 , V 2 O 5 , NH 4 VO 3 ] as a mattress, and a neodymium (Nd) compound and an erbium (Er) compound are mixed as an activator. After the firing time at 600-700 ℃ for 3-5 hours in the oxidizing atmosphere by 1st stage reaction, it is pulverized to the diameter of 5-15μm, and the crushed product is calcined at 1000-12000 ℃ for 3-5 hours after 2 stage reaction. A method for producing an invisible luminescent material, characterized in that the pulverized to a size of about 2-4μm, sintered the second stage reactant at 500-700 ℃ for 1-3 hours and pulverized to about 1μm in a three-step reaction. 특허청구범위의 제2항에 있어서, 산화물인 매트릭스가 Y2SiV2O10인 것을 특징으로 하는 비가시 발광물질의 제조 방법.The method according to claim 2, wherein the matrix, which is an oxide, is Y 2 SiV 2 O 10 . 제2항 또는 제3항에 있어서, 활성화제인 네오디뮴 화합물은 Nd2O3이고, 어븀화합물은 Er2O3인 것을 특징으로 하는 비가시 발광물질의 제조 방법.The method of claim 2, wherein the neodymium compound as an activator is Nd 2 O 3 , and the erbium compound is Er 2 O 3 . 제4항에 있어서, 네오디뮴 화합물인 Nd2O3는 0.001mol이고, 어븀 화합물인 Er2O3는 0.0003mol인 것을 특징으로 하는 비가시 발광물질의 제조 방법.The method of claim 4, wherein the neodymium compound Nd 2 O 3 is 0.001 mol and the erbium compound Er 2 O 3 is 0.0003 mol. 제2항 또는 제3항에 있어서, 활성화제인 네오디뮴 화합물은 Nd의 함량이 매트릭스량의 0.2-0.3%되도록 Nd 화합물[NdCl3, NdF3, (CH3CO2)Nd, Nd(NO3)3, Nd2O3, Nd2(SO4)3]을 혼합한 것이고, 어븀 화합물은 Er의 함량이 매트릭스량의 0.1%되도록 Er 화합물[ErCl3, Er(CO3)3, ErF3, Er(NO3)3, Er2O3]을 혼합하는 것을 특징으로 하는 비가시 발광물질의 제조 방법.The neodymium compound as claimed in claim 2 or 3, wherein the neodymium compound is an Nd compound [NdCl 3 , NdF 3 , (CH 3 CO 2 ) Nd, Nd (NO 3 ) 3 so that the Nd content is 0.2-0.3% of the matrix amount. , Nd 2 O 3 , Nd 2 (SO 4 ) 3 ], and the erbium compound is a mixture of Er compounds [ErCl 3 , Er (CO 3 ) 3 , ErF 3 , Er ( NO 3 ) 3 , Er 2 O 3 ] A method for producing an invisible light emitting material, characterized in that the mixture.
KR1019960045650A 1996-10-14 1996-10-14 Non-visible light-emitting materials and methods for their production KR0178356B1 (en)

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KR101238197B1 (en) * 2010-12-27 2013-02-28 한국조폐공사 Invisible Luminescence Material and Method for Manufacturing The Same
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