CN1297627C - Machine-readable fluorescence/phosphorescence anti false material, method for fabricating the material and application - Google Patents
Machine-readable fluorescence/phosphorescence anti false material, method for fabricating the material and application Download PDFInfo
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- CN1297627C CN1297627C CNB2004100339290A CN200410033929A CN1297627C CN 1297627 C CN1297627 C CN 1297627C CN B2004100339290 A CNB2004100339290 A CN B2004100339290A CN 200410033929 A CN200410033929 A CN 200410033929A CN 1297627 C CN1297627 C CN 1297627C
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- sesquioxide
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Abstract
The present invention relates to a machine readable material which is a powder material prepared by doping other rare earth oxides (RE2O3) in europium oxide (Eu2O3), wherein the ratio of the RE2O3 to the Eu2O3 is (2:1) to (40:1). The average particle diameter of the powder material is smaller than 5 micrometers, the powder material emits red visible fluorescence when the powder material is excitated by short wave ultraviolet rays, and the afterglow life time of the powder material is less than 5 milliseconds. The method comprises the following technological methods: transferring rare earth ions of the rare earth oxides to a liquid phase; separating precipitable salts of rare earth negative ions out of the liquid phase; sintering the precipitable salts into rare earth oxides. The present invention aims at providing a machine readable luminescent material and a preparation method, the machine readable luminescent material is suitable for various ink production technologies and printing conditions and is suitable for print, and the machine readable luminescent material has preferable physics and chemistry resistance, and preferable long-term high energy ultraviolet irradiation resistance property. The machine readable material is especially suitable for identifying and classifying various safety printing products.
Description
Technical field
The present invention relates to a kind of making method and application thereof with machine readable material that is suitable for printing of fluorescence-phosphorescence feature.Specifically, anti-fake material of the present invention is applied on the safe printing such as Valued Securities, has false proof and is convenient to realize the function of machine sorting.
Background technology
In the false proof of safe printings such as Valued Securities and machine sorting, using Ultraluminescence, phosphorescence technology is one of general means.Luminescent material with Ultraluminescence, phosphorescence feature is a lot, the disclosed a kind of matrix material luminous under UV-light of Chinese patent literature CN1332222A for example, this matrix material comprises the negative ion of organic carboxyl acid or derivatives thereof, as: the amino acid of the N-unit acylations that phenylformic acid, phthalic acid, terephthalic acid, Tetra hydro Phthalic anhydride and amino acid reaction produce or organic amide etc.; The rare earth metal terbium ion; Other metal ions with the terbium codoped comprise: cerium, lanthanum or dysprosium; Comprise the alkaline-earth metal or the transition metal ion of calcium, strontium or zinc etc., and comprise polyoxyethylene glycol, Polyvinylpyrolidone (PVP), synthetic glass, the macromolecule dispersant of nylon lamp.Rare earth luminescence has the luminous efficiency height, luminescence spectrum is narrow and characteristics such as energy density height, referring to " coordination chemistry summary " magazine, and the content that 1993 the 123rd volumes are the 201st page.Fluorescent material by the preparation of small molecules rare earth compound, be widely used in aspects such as trichromoscope, luminescent lamp, X-ray intensifying screen, these materials mostly are that inorganic powder or crystal are (referring to " Englishize association will, dalton " magazine, 1996, the 3613rd page).If rare earth metal is incorporated in the polymeric matrix, be prepared into polymkeric substance/rare earth luminous matrix material, have synthetic convenient, forming process is easy, in light weight and low cost and other advantages.But rare earth ion in polymer poor solubility, be difficult for to disperse, take place easily again to assemble and influence luminous efficiency.In order to improve dispersiveness, adopt the method for ligand (ligand) and rare earth metal formation complex compound in recent years, or directly utilization have the method for the Ionomer of complexing action as carrier, (referring to " macromole magazine " nineteen eighty-three, the 16th volume, the 749th page).Simultaneously in actual applications, in order to improve the extinction ability of rare earth ion, also adopted the method for adding sensitizing agent to obtain rare earth one polymer one sensitizing agent three-component compound system, (as " journal of applied " 1992, the 45th volume, the 1641st page report).
But, be suitable for making the few of printing ink and fine realization printing for existing luminescent material.Its main problem is, luminescent material is limit by himself performance, constitutional features, the printing marking is difficult to satisfy the circulation environment requirement of safe printing strictnesses such as Valued Securities to the endurance quality of external environment, as organic fluorescent material system China ink not organic solvent-resistant, poor heat stability; Inorganic fluorescent material is because crystal grain is difficult for the system China ink greatly, and printability is poor, and anti-physical chemistry also has undesirable, as sulfide and the not long-time irradiation of anti-strong UV-light of oxysulfide, along with duration of service its characteristics of luminescence can weaken gradually; Aluminate is not water-fast and particle is thick, and it is configured in when printing in the printing ink, and its crystal grain usually is damaged, thereby destroys its predetermined characteristics of luminescence yet, is not suitable for processing system China ink; In addition, phosphoric acid salt powder homogeneity is bad, luminously is subjected to the influence of lattice imperfection very big; The heat-resisting water of borate is poor, and is very high to temperature control requirement during preparation.In addition, the poor performance of the long-term anti-high energy uviolizing of luminescent material of using in the existing printing.
On the other hand, the twilight sunset life-span of existing most of luminescent material fluorescence is unsuitable for realizing the sorting of safe printing machine by it is detected.
Summary of the invention
For this reason, technical problem to be solved of the present invention is to propose a kind of black technology of various systems and printing condition of being suitable for, and has anti-preferably physics and chemical property, and the application of the luminescent material of long-term preferably anti-high energy uviolizing performance is arranged.
The technical problem of further solution of the present invention is to propose a kind of printing ink or material that safe printing is carried out the machine sorting that be suitable for.
Be above-mentioned technical problem of the present invention, the application of fluorescent/phosphorescent material of the present invention, wherein said fluorescent/phosphorescent material is europium sesquioxide (Eu
2O
3) other rare earth oxide (RE mixes
2O
3) meal formed, the proportion relation of described europium sesquioxide and described other rare earth oxide is:
RE
2O
3∶Eu
2O
3＝2∶1-40∶1
The median size of described meal is less than 4 microns, and it is subjected to the short-wave ultraviolet ray excited red visible fluorescence that sends, and the twilight sunset life-span of described fluorescence is below 5 milliseconds; Described material is used for machine-readable sorting mark.
Wherein, described other rare earth oxide selective oxidation yttrium, Neodymium trioxide, Erbium trioxide, gadolinium sesquioxide, lanthanum trioxide and/or Indium sesquioxide.
The application that contains fluorescent/phosphorescent material printing ink of the present invention, wherein said fluorescent/phosphorescent material is europium sesquioxide (Eu
2O
3) other rare earth oxide (RE mixes
2O
3) meal formed, the proportion relation of described europium sesquioxide and described other rare earth oxide is:
RE
2O
3∶Eu
2O
3＝2∶1-40∶1
The median size of described meal is less than 4 microns, and it is subjected to the short-wave ultraviolet ray excited red visible fluorescence that sends, and the twilight sunset life-span of described fluorescence is below 5 milliseconds; It is characterized in that, be not less than 5% at the content of fluorescent/phosphorescent material described in the described printing ink; Described printing ink is used for machine-readable sorting mark.
Wherein, other rare earth oxide selective oxidation yttrium, Neodymium trioxide, Erbium trioxide, gadolinium sesquioxide, lanthanum trioxide and/or Indium sesquioxide.
Technique scheme of the present invention has the following advantages compared to existing technology: the median size that adopts the machine readable anti-fake material that is suitable for printing that above-mentioned making method produces is less than 4 microns, and it is configured in the requirement that can satisfy flat stamping, protruding seal, gravure ink in the printing ink.During printing, its crystal grain is difficult for being damaged, thereby can satisfy its predetermined characteristics of luminescence.By the group mode of machine readable anti-fake material of the present invention, it is short-wave ultraviolet ray excited to cause described machine readable material to be subjected to, and can send the twilight sunset life-span at the red visible fluorescence below 5 milliseconds.Have good chemical-resistant stability and weathering resistance, can satisfy the circulation requirement of safe printing strictness; More usable time is done the parameter of signal, improves machine-readable safe dynamics.
Embodiment
For the easier quilt of content of the present invention is clearly understood, the present invention is further detailed explanation according to a particular embodiment of the invention below.
Embodiment 1
In the present embodiment, get yttrium oxide (Y
2O
3) and europium sesquioxide (Eu2O3) in the preparation of 2 to 1 ratio, the material after the preparation is dissolved in the hydrochloric acid (HCl), form the rare earth chloride of europium and yttrium.The rare earth chloride of europium and yttrium is prepared into the rare-earth oxalate of europium and yttrium.Then, to the capable calcination of rare-earth oxalate of europium and yttrium, calcination temperature is got 1000 degrees centigrade, and calcination time is more than 1 hour.Make the meal of europium sesquioxide doped yttrium oxide thus, the median size of this meal is less than 4 microns, is being subjected to send red visible fluorescence, and the twilight sunset life-span of described fluorescence being below 5 milliseconds when short-wave ultraviolet ray excited.
The meal of europium sesquioxide doped yttrium oxide is added in the printing ink, make fluorescent ink.Described fluorescent ink is imprinted on the marking on the safe printing such as Valued Securities, can be used as anti-counterfeiting mark, also can be used as the signal generating source of realizing the machine sorting.The source takes place sort signal both can be used for the real-time signal detection, also can be used for inhibit signal and detected.
In the fluorescent ink, the meal of described europium sesquioxide doped yttrium oxide accounts for 5% of weight as described, and this fluorescent ink is printed on the safe printing, is formed on the colourless marking of launching red fluorescence under the exciting of short wave ultraviolet.
As described in the fluorescent ink, the meal of described europium sesquioxide doped yttrium oxide accounts for 5% of weight, simultaneously colored pigment accounts for 10% of weight, and this fluorescent ink is printed on the safe printing, is formed on coloured marking of launching red fluorescence under the exciting of short wave ultraviolet.
As described in the fluorescent ink, the meal of described europium sesquioxide doped yttrium oxide accounts for 10% of weight, long wave ultra-violet light-emitting fluorescence branch accounts for the 1-10% of weight simultaneously, this fluorescent ink is printed on the safe printing, forming it is lacking, during the irradiation respectively of long wave ultraviolet, is launching red under the shortwave or fluorescent orange and the long wave fluorescence of other color of emission down.
Embodiment 2
In the present embodiment, the yttrium oxide among the embodiment 1 replaces with gadolinium sesquioxide, and gadolinium sesquioxide and europium sesquioxide are in 20 to 1 ratio preparation.Enter liquid phase-commentaries on classics rare-earth oxalate at above-mentioned rare earth oxide-commentaries on classics rare earth ion and separate out-be sintered to oxide compound from liquid phase, wherein calcination temperature is got 800 degrees centigrade.Identical among other making processes and the embodiment 1.The meal median size of the europium sesquioxide doping gadolinium sesquioxide of making is less than 4 microns, is being subjected to send red visible fluorescence, and the twilight sunset life-span of described fluorescence being below 4 milliseconds when short-wave ultraviolet ray excited.Identical among the effect of the meal of europium sesquioxide doping gadolinium sesquioxide and application mode and the embodiment 1.
Embodiment 3
In the present embodiment, the yttrium oxide among the embodiment 1 replaces with lanthanum trioxide, and lanthanum trioxide and europium sesquioxide are in 10 to 1 ratio preparation.Enter liquid phase-commentaries on classics rare-earth oxalate at above-mentioned rare earth oxide-commentaries on classics rare earth ion and separate out-be sintered to oxide compound from liquid phase, wherein calcination temperature is got 900 degrees centigrade.Identical among other making processes and the embodiment 1.The meal median size of the europium sesquioxide doping lanthanum oxide of making is less than 4 microns, is being subjected to send red visible fluorescence, and the twilight sunset life-span of described fluorescence being below 4 milliseconds when short-wave ultraviolet ray excited.Identical among the effect of the meal of europium sesquioxide doping lanthanum oxide and application mode and the embodiment 1.
Embodiment 4
In the present embodiment, the yttrium oxide among the embodiment 1 replaces with Indium sesquioxide, and Indium sesquioxide and europium sesquioxide are in 5 to 1 ratio preparation.Enter liquid phase-commentaries on classics rare-earth oxalate at above-mentioned rare earth oxide-commentaries on classics rare earth ion and separate out-be sintered to oxide compound from liquid phase.Identical among other making processes and the embodiment 1.The meal median size of the europium sesquioxide doped indium oxide of making is less than 4 microns, is being subjected to send red visible fluorescence, and the twilight sunset life-span of described fluorescence being below 4 milliseconds when short-wave ultraviolet ray excited.Identical among the effect of the meal of europium sesquioxide doped indium oxide and application mode and the embodiment 1.
Embodiment 5
In the present embodiment, the yttrium oxide among the embodiment 1 replaces with Neodymium trioxide, and Neodymium trioxide and europium sesquioxide are prepared in 5 to 1 ratio.Enter liquid phase-commentaries on classics rare-earth oxalate at above-mentioned rare earth oxide-commentaries on classics rare earth ion and separate out-be sintered to oxide compound from liquid phase.Identical among other making processes and the embodiment 1.The meal median size of the europium sesquioxide doping neodymium oxide of making is less than 4 microns, is being subjected to send red visible fluorescence, and the twilight sunset life-span of described fluorescence being below 4 milliseconds when short-wave ultraviolet ray excited.Identical among the effect of the meal of europium sesquioxide doping neodymium oxide and application mode and the embodiment 1.
Embodiment 6 in the present embodiment, the yttrium oxide among the embodiment 1 replaces with Erbium trioxide, and Erbium trioxide and europium sesquioxide are in the preparation of 10 to 1 ratio.Enter liquid phase-commentaries on classics rare-earth oxalate at above-mentioned rare earth oxide-commentaries on classics rare earth ion and separate out-be sintered to oxide compound from liquid phase.Identical among other making processes and the embodiment 1.The meal median size of the europium sesquioxide doping Erbium trioxide of making is less than 4 microns, is being subjected to send red visible fluorescence, and the twilight sunset life-span of described fluorescence being below 4 milliseconds when short-wave ultraviolet ray excited.Identical among the effect of the meal of europium sesquioxide doped yttrium oxide and application mode and the embodiment 1.
In embodiments of the present invention, the rare earth based material also can adopt two or more rare earth compound.Under prompting of the present invention, the person of ordinary skill in the field selects for use two or more rare earth compounds as substrate material according to known general knowledge, and resulting effect is conspicuous.
Because rare earth compound of the present invention has roughly the same characteristic, therefore the choosing of parameters in the preparation process of the meal of described machine readable anti-fake material of the present invention also is roughly the same.In the above-described embodiments, selected parameter difference among the different embodiment, and do not mean that this parameter and corresponding embodiment's is corresponding.Be interpreted as these parameters and also can replacedly adopt in other embodiments, and can obtain the effect that can realize the object of the invention.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And these belong to conspicuous variation or the change that spirit of the present invention extended out and still are among protection scope of the present invention.
Claims (4)
1. the application of a fluorescent/phosphorescent material, wherein said fluorescent/phosphorescent material is europium sesquioxide (Eu
2O
3) other rare earth oxide (RE mixes
2O
3) meal formed, the proportion relation of described europium sesquioxide and described other rare earth oxide is:
RE
2O
3∶Eu
2O
3＝2∶1-40∶1
The median size of described meal is less than 4 microns, and it is subjected to the short-wave ultraviolet ray excited red visible fluorescence that sends, and the twilight sunset life-span of described fluorescence is below 5 milliseconds; It is characterized in that described material is used for machine-readable sorting mark.
2. the application of fluorescent/phosphorescent material according to claim 1 is characterized in that, described other rare earth oxide selective oxidation yttrium, Neodymium trioxide, Erbium trioxide, gadolinium sesquioxide, lanthanum trioxide and/or Indium sesquioxide.
3. application that contains fluorescent/phosphorescent material printing ink, wherein said fluorescent/phosphorescent material is europium sesquioxide (Eu
2O
3) other rare earth oxide (RE mixes
2O
3) meal formed, the proportion relation of described europium sesquioxide and described other rare earth oxide is:
RE
2O
3∶Eu
2O
3＝2∶1-40∶1
The median size of described meal is less than 4 microns, and it is subjected to the short-wave ultraviolet ray excited red visible fluorescence that sends, and the twilight sunset life-span of described fluorescence is below 5 milliseconds; It is characterized in that, be not less than 5% at the content of fluorescent/phosphorescent material described in the described printing ink; Described printing ink is used for machine-readable sorting mark.
4. the application that contains fluorescent/phosphorescent material printing ink according to claim 3 is characterized in that, described other rare earth oxide selective oxidation yttrium, Neodymium trioxide, Erbium trioxide, gadolinium sesquioxide, lanthanum trioxide and/or Indium sesquioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100339290A CN1297627C (en) | 2004-04-20 | 2004-04-20 | Machine-readable fluorescence/phosphorescence anti false material, method for fabricating the material and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100339290A CN1297627C (en) | 2004-04-20 | 2004-04-20 | Machine-readable fluorescence/phosphorescence anti false material, method for fabricating the material and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1563270A CN1563270A (en) | 2005-01-12 |
| CN1297627C true CN1297627C (en) | 2007-01-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100339290A Expired - Fee Related CN1297627C (en) | 2004-04-20 | 2004-04-20 | Machine-readable fluorescence/phosphorescence anti false material, method for fabricating the material and application |
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| CN (1) | CN1297627C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102010026627A1 (en) * | 2010-07-09 | 2012-01-12 | Giesecke & Devrient Gmbh | Alkali metal and alkaline earth metal niobates and tantalates as security feature substances |
| CN102909988B (en) * | 2012-10-31 | 2015-01-21 | 中国人民银行印制科学技术研究所 | Valuable document and identification method thereof |
| BR112015031499A2 (en) * | 2013-06-19 | 2017-07-25 | K Fee System Gmbh | single dose capsule with fluorescent and / or phosphorescent identification |
| CN108944149A (en) * | 2018-06-29 | 2018-12-07 | 华南理工大学 | A kind of valuable document and the method for verifying its true and false |
| CN111040516A (en) * | 2019-12-30 | 2020-04-21 | 天津市中环天佳电子有限公司 | Rare-earth anti-fake inkpad |
| CN111103774A (en) * | 2019-12-31 | 2020-05-05 | 天津市中环天佳电子有限公司 | Printer powdered ink of rare earth spectrum tracing |
| CN111077746A (en) * | 2019-12-31 | 2020-04-28 | 天津市中环天佳电子有限公司 | Rare earth spectrum traceable ink powder for golden light red printer |
| CN117936254A (en) * | 2024-03-25 | 2024-04-26 | 淄博益久塑胶有限公司 | Preparation method of magnetic raw material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064301A (en) * | 1991-12-28 | 1992-09-09 | 上海跃龙有色金属有限公司 | High quality red fluorescent powder and manufacturing process thereof |
| JP2000256591A (en) * | 1999-03-09 | 2000-09-19 | Hitachi Maxell Ltd | Fluorescent pigment ink and its production |
| CN1297964A (en) * | 1999-11-30 | 2001-06-06 | 上海跃龙有色金属有限公司 | Preparation of red phosphor |
-
2004
- 2004-04-20 CN CNB2004100339290A patent/CN1297627C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064301A (en) * | 1991-12-28 | 1992-09-09 | 上海跃龙有色金属有限公司 | High quality red fluorescent powder and manufacturing process thereof |
| JP2000256591A (en) * | 1999-03-09 | 2000-09-19 | Hitachi Maxell Ltd | Fluorescent pigment ink and its production |
| CN1297964A (en) * | 1999-11-30 | 2001-06-06 | 上海跃龙有色金属有限公司 | Preparation of red phosphor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1563270A (en) | 2005-01-12 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Inst. of Printing Science, Peolpe's Bank of China Assignor: China banknote printing and Minting Corporation Contract fulfillment period: 2008.11.11 to 2013.11.10 contract change Contract record no.: 2008110000159 Denomination of invention: Machine-readable fluorescence/phosphorescence anti false material, method for fabricating the material and application Granted publication date: 20070131 License type: Exclusive license Record date: 2008.12.5 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.11.11 TO 2013.11.10; CHANGE OF CONTRACT Name of requester: PEOPLE'S BANK OF CHINA SCIENCE PRINTING TECHNOLOGY Effective date: 20081205 |
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Granted publication date: 20070131 Termination date: 20170420 |