CN108918485A - Method for anti-counterfeit, corresponding drug, anti-counterfeiting ink and application based on Nano diamond - Google Patents
Method for anti-counterfeit, corresponding drug, anti-counterfeiting ink and application based on Nano diamond Download PDFInfo
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- CN108918485A CN108918485A CN201810596673.6A CN201810596673A CN108918485A CN 108918485 A CN108918485 A CN 108918485A CN 201810596673 A CN201810596673 A CN 201810596673A CN 108918485 A CN108918485 A CN 108918485A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06K—GRAPHICAL DATA READING; PRESENTATION OF DATA; RECORD CARRIERS; HANDLING RECORD CARRIERS
- G06K7/00—Methods or arrangements for sensing record carriers, e.g. for reading patterns
- G06K7/10—Methods or arrangements for sensing record carriers, e.g. for reading patterns by electromagnetic radiation, e.g. optical sensing; by corpuscular radiation
- G06K7/14—Methods or arrangements for sensing record carriers, e.g. for reading patterns by electromagnetic radiation, e.g. optical sensing; by corpuscular radiation using light without selection of wavelength, e.g. sensing reflected white light
- G06K7/1404—Methods for optical code recognition
- G06K7/1439—Methods for optical code recognition including a method step for retrieval of the optical code
- G06K7/1447—Methods for optical code recognition including a method step for retrieval of the optical code extracting optical codes from image or text carrying said optical code
Abstract
The invention discloses a kind of method for anti-counterfeit based on Nano diamond, corresponding drug, anti-counterfeiting ink and applications, wherein the method for anti-counterfeit based on Nano diamond is the surface coated with nano diamond particles by the article to pending anti-fake processing, either by mixing Nano diamond particle inside the article to pending anti-fake processing, contain nitrogen-vacancy center NV in negative charge state inside these Nano diamond particles‑, using these Nano diamond particles in the case where wavelength is the excitation of 400nm~600nm the fluorescence that issues, carry out anti-fake.The present invention chooses internal nitrogen-vacancy center NV containing in negative charge state by controlling crucial its internal structure of Nano diamond material‑Nano diamond material can effectively be realized anti-fake using fluorescent characteristic of the Nano diamond material under 400nm~600nm wavelength (especially 532nm wavelength) exciting light.
Description
Technical field
The invention belongs to field of anti-counterfeit technology, more particularly, to a kind of method for anti-counterfeit based on Nano diamond, phase
Drug, anti-counterfeiting ink and application are answered, which can be applied to anti-forgery ink, anti-forge paper, Drug Authentication, can accordingly obtain
To anti-counterfeiting ink and the drug through anti-fake processing.
Background technique
Conventional anti-forgery ink is mainly the following classification：Fluoresent printing ink, daylight excitation color shifting ink, infrared
Anti-forgery ink, temperature-sensitive anti-forgery ink, pressure-sensitive anti-forgery ink, magnetic anti-forge printing ink, optically variable security ink, anti-correction are anti-fake
Ink.These three ink (are referred to as discoloration oil below by fluoresent printing ink, daylight excitation color shifting ink, Antiforge infrared ink
Ink) be all under the irradiation of light issue visible light obtain ink, the corresponding light of these three ink be respectively ultraviolet light, sunlight,
Infrared light.The basic principle is that special material is added in coloured or colorless ink, this special material can be specific
Launch the light of certain special wavelength under the irradiation of light.The luminescent material added in existing color shifting ink is carbon quantum dot
(CN107057463A), graphene quantum dot (CN106752380A), silicon quantum dot (CN105086628A), ZnO quantum dot
(CN103289469A),ZnS:Mn/ZnS (CN10307946A), nanometer ZnS/nano-ZnO (CN05482551A), Y2O3:Eu,
Er (CN103113784A), nitrogen carbide quantum dot (CN104861784B), dichlorofluorescein (CN103849217A), NaYF4:
Yb,Er,NaYF4:Yb,Tm,NaYF4:Er, Tm nanoparticle (CN104371424A), nitrogen mix carbon nano-particles
(CN103113886A), Eu, Dy, Tb (US005837042A), Eu, Tb, Sm, Dy, Lu, Ln, Gd (US005525798A) etc.
Deng.
Material of the above for anti-forgery ink is first in addition to carbon quantum dot, silicon quantum dot, nitrogen carbide quantum dot have had
Step prove it is non-hazardous to human body at low concentrations other than[1][2][3], it is malicious to there is a degree of biology in remaining material
Property[4][5][6][7][8], and some materials are because self character leads to photobleaching[9][10][11], and the fluorescence under the irradiation of light
The fluorescence intensity that matter is ejected gradually weakens or even disappears as time goes by.
Nano diamond containing nitrogen-vacancy center (Nitrogen-vacancy center, NV center), has
The physical properties such as hardness is big, optical clear is high pressure resistant, weathering resistance, and have good biocompatibility, hypotoxicity and unglazed
Cause the characteristics such as bleaching[12][13][14][15].The center NV is mainly with NV0And NV-Two kinds of state of charge exist, what general experiment was used
It is all NV-。NV-Electronic structure in include six electronics two of them electronics be to be provided by nitrogen-atoms, three electronics come from
Three carbon atoms in hole are centered around, and another electronics is captured from the lattice of nitrogen-atoms.Except special in the present invention
Outside illustrating, the center NV refers to NV-State.At present containing the centrical Nano diamond with photoluminescent property of nitrogen-sky
(hereinafter referred to as fluorescence diamond) has many applications in biological field[16], as the isolation and purification of protein, cell marking with
Bio-imaging, bio-sensing, gene delivery and treatment, drug delivery and treatment, cancer diagnosis and treatment, enhancing immunocompetence
Etc..
With traditional Nano diamond the difference is that its internal nitrogen-vacancy central defect structure (see Figure 1A), is somebody's turn to do
Structure is a kind of common defects in diamond, is the nitrogen-atoms and adjacent lattice by replacing carbon atom in lattice
A vacancy on point is constituted, and possesses unique level structure and optical property, specific wavelength (especially in 500nm it is attached
Can inspire highly stable fluorescence under laser irradiation closely), fluorescent wavelength ranges in 550nm between 800nm, color master
It will be based on red.
Common diamond is the clear crystal being made of simple carbon, that is, the diamond being commonly called as, every in crystal
A carbon atom is all with sp3The hybridized orbit carbon atom composition covalent bond adjacent with four additional is mesh because of its stable structure
The most hard substance of preceding known naturally occurring, and without any fluorescent effect, thermal conductivity are high so common diamond
Sand paper, probing are generally used for, on milling tool, for cutting and portraying the heat dissipations such as other substances, and large-scale integrated circuit
On plate, also there is the value as craftwork certainly.But this common diamond without NV structure is not due to having fluorescence
Effect, therefore it is not used to anti-counterfeit field.
The application of NV Nano diamond is concentrated mainly on aspect related with magnetic-field measurement, the shadow using NV in magnetic field at present
Ring the characteristic that its lower fluorescence can change, can be used for magnetic-field measurement (WO2016126436A1, US8947080B2,
US20170211947), magnetic target acquisition (US20170343699A1), biomarker (US20050019955), also utilization
NV characteristic is to realize single-photon source (US20090034737).Its principle of technology in relation to magnetic detection is, when NV Nano diamond
In the case where there is magnetic field, internal energy level has certain variation, to will affect its fluorescent brightness.According to fluorescence
Variation can release the property in magnetic field.
And on the other hand, on Drug Authentication, according to the World Health Organization 2017 publication a survey report table
It is bright[17], in the sampling Detection of drug, about 10.5% counterfeit drug in low income country, middle income country's counterfeit drug rate is
10.6%.This will lead to serious consequence, and by taking children Streptococcus as an example, if counterfeit drug can cut down a part of antibody vigor, that can be led
Children dead due to pneumonia more than 70,000 are caused, that there will be 170,000 children because pneumonia is dead if counterfeit drug can completely inhibit antibody activity
It dies.
Global counterfeit drug consumption sum is more than 50,000,000,000 dollars within 2010, and the counterfeit drug sales volume in the whole world is just with annual 15%
Speed increase[18]。
The problem of corresponding i.e. anti-drug counterfeiting, the anti-fake of drug at present tend to using Components identification method, by with
The ingredient of standard pharmaceutical compares to distinguish authenticity of medicament.Nat'l Pharmaceutical & Biological Products Control Institute sets up special scientific research within 2003
Group carries out the research of drug rapid detection system, and whole system can be summarized as two technology platforms at present：(1) it is examined with drug
Measuring car is the quick initial screening platform of medicine on-site of carrier, the laboratory Rapid Confirmation platform of (2) based on authorization method.
The former is mainly equipped with near-infrared rapid detection system and the quick identification system of chemistry, compounding chemicals information management system, benefit
Good with vehicular movement, near-infrared analysis is quick, undamaged feature, realize adulterated drug is carried out at base scene it is quick
Experiment screening, with the frequency and density for improving supervision, checking, drugs monitoring vehicle will be provided to the prefectures and cities in the whole nation.The latter is main
Including HPLC rapid measuring system and LC-MS quick analysis system, HPLC rapid measuring system is mainly equipped on prefectures and cities' medicine inspection
Institute, LC-MS quick analysis system are then grasped by each provincial medicine inspecting institute or regional emphasis medicine inspecting institute.
The wave-length coverage of near-infrared (Near infrared, NIR) spectrum is 780-2526nm, and that predominantly detect is O-
H, the frequency multiplication of the hydric groups vibrational spectrum such as N-H, C-H, S-H and sum of fundamental frequencies absorb, but because its bands of a spectrum is wide, overlapping is more serious,
And absorption signal is weak, information parsing complexity and other reasons leads to its measurement accuracy or there is a certain error, is only suitable for using
In doing quick detection.
HPLC (High performance liquid chromatography, high pressure liquid chromatography) method is chromatography
An important branch, using liquid as mobile phase, using high pressure transfusion system, by the single solvent with opposed polarity or not
The mobile phases such as mixed solvent, buffer in proportion are pumped into the chromatographic column equipped with stationary phase, after each ingredient is separated in column,
It is detected into detector, to realize the analysis to sample.Although this method has greatly facilitated medicine inspecting institute of base
Quick detection to adulterated drug, but still require that each medicine inspecting institute of base saves all drug reference substances, still have one at present
Fixed difficulty, therefore it is still limited by reference substance.
LC-MS (Liquid chromatography-mass spectrometry, liquid chromatograph mass spectrography) is one
The technique of analytical chemistry that kind combines the physical separation ability of high performance liquid chromatography and simple mass analyzing capability, tool
There are very high susceptibility and selectivity.The key for establishing LC-MS authorization method is to establish the standard matter of homology drug
Library is composed, and is able to satisfy different model, the public LC-MS standard mass spectral database that the mass spectrograph of producer is retrieved, compared, judged, is
Guarantee that different experiments room LC-MS plays the key of maximal efficiency.
Other than the method directly analyzed drug ingredient, also has and anti-fake mark is carried out to reality to drug
It now can be with the scheme of Rapid identification.RFID (Radio is utilized in GlaxoSmithKline company on its product within 2006
Frequency identification, radio frequency identification) technology will be at medicine box (medicine bottle) after production line under drug
Bottom patch plus RFID tag, inside tags contain ID coding, this coding has uniqueness, can allow retailer and medicine
Product user verifies the true and false of drug, and drug retail trader can also carry out effective monitoring to drug in supply chain[19], also have
The means (CN105818559A) that Key works Drug packing is processed by laser anti-counterfeiting.
Although but method accurate still realization complexity, the common people that the former carries out constituent analysis to drug will pass through this
Kind of mode carry out drug identification needs devote considerable time, energy.And the latter is although convenient and efficient, but only to package medicine
The packaging of object is marked, if fake and inferior drug is put into regular packaging, then the method is helpless.
At the same time, the intake ability and nanogold for thering is team to have studied different types of cell to Nano diamond
Influence of the hard rock to cell division and atomization[20], the experimental results showed that carboxyl Nano diamond is in cell division and differentiation
In the process without toxicity, it does not change the level of Cell growth ability and cell cycle mediating proteins.In cell mitogen
In the process, Nano diamond do not interfere not only spindle formation and chromosome and separate, but also can approximately be divided into
Two halves are into each daughter cell.There are also very for safety research about Nano diamond to cell, biology
It is more[13][14][15][21][22], it is that one kind can be used safely in the outstanding of biological, medical aspect that they, which also show Nano diamond,
Material.Particularly there is team using nitrogen-vacancy center fluorescent characteristic in Nano diamond at present, has developed it in nuclear-magnetism
In terms of resonance image-forming[23][24][25][26][27]And the application of the thermometer as cell interior[28].Bibliography：
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Modules-SPC
M.aspx
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the purpose of the present invention is to provide one kind to be based on nanogold
The method for anti-counterfeit of hard rock, corresponding drug, anti-counterfeiting ink and application, wherein by crucial Nano diamond material inside it
Structure is controlled, and internal nitrogen-vacancy center NV containing in negative charge state is chosen-Nano diamond material, utilize this
Fluorescent characteristic of the Nano diamond material under the nm of 400nm~600 wavelength (especially 532nm wavelength) exciting light, can be effective
It realizes anti-fake, gives a kind of new method for anti-counterfeit compared to the prior art；Also, it is nontoxic due to Nano diamond material
Property, biocompatibility the features such as so that should method for anti-counterfeit based on Nano diamond can be applied to anti-drug counterfeiting, and it is corresponding
It obtains carrying anti-fraud functional drug；In addition, the present invention also by grain diameter to Nano diamond, inside NV- it is dense
Degree etc. is preferably controlled, and Nano diamond grain diameter is controlled as 5nm~500nm, and by Nano diamond material internal
NV-It is 10ppm to 100ppm that concentration, which further preferably controls, the fluorescence signal of Nano diamond can be made more obvious, by force
Degree is reinforced, the more conducively clear identification of anti-counterfeiting signal, makes method for anti-counterfeit and application more accurate and effective in the present invention.
To achieve the above object, according to one aspect of the present invention, a kind of anti-fake side based on Nano diamond is provided
Method, which is characterized in that this method is the surface coated with nano diamond particles by the article to pending anti-fake processing, or
Person is by mixing Nano diamond particle inside the article to pending anti-fake processing, inside these Nano diamond particles
Contain the nitrogen-vacancy center NV for being in negative charge state-, using these Nano diamond particles wavelength be 400nm~600nm
Excitation under the fluorescence that issues, carry out anti-fake；Preferably, the partial size of these Nano diamond particles be 5nm~
500nm, inside contained by NV-Concentration control is 10ppm to 100ppm.
It is by the table to article to be detected or article to be detected when detecting as present invention further optimization
Face or article to be detected crush composition granule or solute is that application wavelength is in the solution of article crushing composition granule to be detected
The exciting light of 400nm~600nm carries out anti-fake then by detecting whether to inspire fluorescence；
When not detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is fakement；
When detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is genuine piece.
As present invention further optimization, the Detection wavelength of the fluorescence is greater than 600nm；
Preferably, the wavelength of the exciting light is 532nm；The Detection wavelength of the fluorescence is preferably greater than 600nm and small
In equal to 800nm.
As present invention further optimization, the article of the pending anti-fake processing is drug.
It is another aspect of this invention to provide that the present invention provides a kind of drug anti-fake based on Nano diamond, feature
It is, is coated with Nano diamond particle on the surface of the drug, or in the inside of the drug include Nano diamond
Grain, the nitrogen in negative charge state-vacancy center NV is contained in the inside of these Nano diamond particles-, for being in wavelength
Fluorescence is issued under the excitation of the exciting light of 400nm~600nm, is carried out anti-fake；Preferably, the grain of these Nano diamond particles
Diameter is 5nm~500nm, NV contained by inside-Concentration control is 10ppm to 100ppm.
As present invention further optimization, the Nano diamond particle is coated in the drug by edible glue
Surface；Preferably, the Nano diamond particle is in the form of the pattern being pre-designed or the pattern of random distribution formation arranges
On the surface of the drug, the pattern being pre-designed is more preferably bar code pattern or pattern in 2 D code, the bar code figure
Case or pattern in 2 D code are for associated with the information of tracing to the source of the drug.
Another aspect according to the invention, the present invention provides a kind of anti-counterfeiting ink based on Nano diamond, features
It is, which includes Nano diamond particle, and the inside of these Nano diamond particles is contained in negative charge state
Nitrogen-vacancy center NV-, for issuing fluorescence under the excitation for the exciting light that wavelength is the nm of 400nm~600, carry out anti-fake；
Preferably, the partial size of these Nano diamond particles is 5nm~500nm, NV contained by inside-Concentration control is arrived for 10ppm
100ppm。
As present invention further optimization, the wavelength of the fluorescence is 550nm~800nm, preferably greater than 600nm
And it is less than or equal to 800nm；
Preferably, the wavelength of the exciting light is 532nm.
It is another aspect of this invention to provide that the present invention provides above-mentioned based on the anti-counterfeiting ink of Nano diamond anti-fake
In application.
As present invention further optimization, the application is specifically to apply to the surface of the article of pending anti-fake processing
Anti-counterfeiting ink is write, is swashed using Nano diamond particle contained by the anti-counterfeiting ink in wavelength for 400 nm~600nm exciting light
The fluorescence of sending is given, is carried out anti-fake；
Preferably, when detecting, by applying the excitation that wavelength is 400nm~600nm on the surface of article to be detected
Light carries out anti-fake then by detecting whether to inspire fluorescence；
When not detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is fakement；
When detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is genuine piece.
Contemplated above technical scheme through the invention, compared with prior art, due to crucial Nano diamond
Its internal structure of material is controlled, and internal nitrogen-vacancy center NV containing in negative charge state is chosen-Nano diamond
Material, it is special using fluorescence of the Nano diamond material under 400nm~600nm wavelength (especially 532nm wavelength) exciting light
Property, it can effectively realize anti-fake, provide a kind of novel anti-fake mode.The present invention is also preferred by carrying out to detection process
Control is the exciting light of 400nm~600nm by applying wavelength, and detects whether to inspire fluorescence (the detection wave band of fluorescence
The preferably greater than wave band of 600nm, such as larger than 600nm and the wave band for being less than or equal to 800nm；It is of course also possible to by 550nm~
600nm or in which some section cover in fluorescence detection wave band), carry out it is anti-fake, do not detect that fluorescence is then fakement,
Detect that fluorescence is then genuine piece.
Contain the nitrogen in negative charge state-vacancy center NV in inside of the present invention-Nano diamond particle,
Its partial size is preferably 5nm~500nm, on the one hand can either ensure to be effectively formed NV-, on the other hand in view of due to excessive
Particle can just may have an impact to human body, and the intensity that its bigger Internal Fluorescent of diamond particles comes out is lower, because
The partial size of this Nano diamond particle used is 5nm~500nm.In addition, the concentration of Nano diamond will affect macro-scale
On luminous intensity, and NV in Nano diamond-Concentration then will affect the luminous intensity of single Nano diamond, the present invention is excellent
It selects NV contained by Nano diamond particle inside-Concentration control is 10ppm to 100ppm, can effectively ensure Nano diamond
Luminous intensity, practical fluorescence detection when convenient for Application in Anti-counterfeiting.
The present invention is to be based on containing the centrical Nano diamond of nitrogen-sky, with fluorescent effect and fluorescent stabilization, and
And property nontoxic to the human body, thus obtained being applied particularly to anti-fake solution, Drug Authentication, ink are anti-fake, screen is anti-fake,
Method for anti-counterfeit in anti-forge paper etc..And because nano diamond structure is stablized, long-term place not will lead to fluorescent functional
It loses, and does not have the appearance of photobleaching phenomenon.
By taking anti-forgery ink as an example, the anti-forgery ink formed using the method in the present invention is had non-toxic to humans
Feature, the anti-forgery ink is similar with traditional color shifting ink, can be in the photograph of the light of specific wavelength (such as 400nm~600nm)
It penetrates down and inspires the light of another special wavelength (wavelength meets 550nm~800nm, especially greater than 600nm, such as larger than 600nm
And it is less than or equal to 800nm).
The present invention can also utilize good biocompatibility, hypotoxicity and the fluorescent characteristic of Nano diamond, in drug
Suitable Nano diamond is added or Nano diamond is sticked to drug substance surface, utilizes the fluorescent characteristic of these Nano diamonds
Carry out anti-fake mark.The present invention passes through the starting point that is added to Nano diamond in common drug as anti-fake marker
It is exactly its chemical inertness, stability, biocompatibility, nontoxicity[29].Its chemical inertness, stability make Nano diamond
The function of drug can't be reacted, influenced with drug, and biocompatibility, nontoxicity make Nano diamond with drug
Into after human body, can't do harm to huamn body.In addition, the present invention further preferably uses edible glue (can certainly use
Other auxiliary, nontoxic reagent with stickiness, safe to the human body) Nano diamond is sticked to drug substance surface, it can make
Naked eyes are invisible after Nano diamond is pasted up, and can not be told truth from falsehood by tactile, to further utilize nanogold
The fluorescent characteristic of hard rock carries out anti-fake.
Detailed description of the invention
Figure 1A is diamond nitrogen-centrical structural schematic diagram of sky, and Figure 1B is that diamond nitrogen-centrical energy level of sky shows
It is intended to.
Fig. 2 is to generate fluorescence schematic diagram.
Fig. 3 is NV-Emission spectrum.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments,
The present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain this hair
It is bright, it is not intended to limit the present invention.In addition, technology involved in the various embodiments of the present invention described below is special
Sign can be combined with each other as long as they do not conflict with each other.
It is right for the applications such as anti-fake by solution separately below, ink is anti-fake, screen is anti-fake, Drug Authentication, anti-forge paper
The present invention is described in detail.It can be 5nm -500nm Nano diamond powder by partial size by spy when anti-fake applied to solution
Certainty ratio (such as extra fine quality percentage concentration) is mixed with target solution, does not need other operations.
Embodiment 1
It, can also be by by nanometer Buddha's warrior attendant by using containing nitrogen-sky centrical Nano diamond realization Drug Authentication
Stone medical surfaces draw figure (these figures either the pattern being pre-designed, such as bar code, two dimensional code, can also be with
Random figure), by the parsing to the figure, authenticity of medicament can be confirmed.With by Nano diamond medical surfaces draw with
For machine figure, method for anti-counterfeit can specifically include following steps：
Step 1：Determine that some region is safety label object area on drug.
Step 2：Nano diamond powder is loaded into spray gun, NV is sprayed on drug-Nano diamond powder,
Medical surfaces form the random figure being made of fluorescence diamond.The adhering mode of powder can be varied, for example, can be with
In the attached one layer of edible glue of drug substance surface, then fill-before-fire NV Nano diamond powder.
Step 3：Sample is received by the laser irradiation drug substance surface of 532nm, and using filter plate, optical signal collection system
Product reflection and the optical signal generated (add filter plate that can filter out the 532nm laser applied by us, only retain such as 600nm
Above light).
Since the fluorescence of generation its intensity is not as good as natural light, it is contemplated that the interference for avoiding natural light is receiving fluorescence signal
When, it can be received (such as in darkroom) under the conditions of being protected from light.
Step 4：By handling the optical signal being collected into, the image of fluorescence signal is obtained.Fluorescent image is pressed
It is divided into zonule one by one according to specific interval, by judging to have in zonule phosphor dot come to zonule assignment 0 or 1, or
Person assigns other values according to fluorescence intensity.The image of obtained transcoding is the identification code of the drug, and server/data are arrived in storage
In library.
Step 5：When needing to carry out anti-counterfeiting detection to drug (before such as medical procurement or before use), by drug table
Face safety label object area carries out fluorescence imaging, and obtaining data comparison in its identification code, with database can determine the true and false.
The present invention can be by Nano diamond particle in the form of bar code pattern or pattern in 2 D code or random distribution is formed
Pattern or other specific patterns (such as other modes that information is converted to figure) arrangements be coated in surfaces of drug.With
Machine figure can be associated with the information of tracing to the source of drug, to distinguish the true and false of drug.Anti-fake figure is bar code pattern or two
The pattern that dimension code pattern etc. is pre-designed is also similar, can use above-mentioned method for anti-counterfeit, wherein step 4 can needed to drug
Operated when anti-counterfeiting detection, these bar codes or two dimensional code can also be linked to the information of tracing to the source of drug.The letter traced to the source
Breath, may include the information such as manufacturer, date of manufacture, also may include formula information, operation instruction information of drug etc. its
His information.
Embodiment 2
By realizing that translucent material forms or include translucent material using containing the centrical Nano diamond of nitrogen-sky
Article (e.g., showing screen etc.) is anti-fake can be using any one in following two scheme：
Scheme one
The program one may include following steps：
Step 1：Article for certain type of transparent material composition or comprising a part of translucent material generates its spy
(this image may include the information of the transparent material or article, can be with for showing screen for different marker graphic pattern
Containing such as screen name, date of manufacture, coding, hardness etc. information), at the same the figure and it includes information storage to service
In device.
Step 2：The a certain region utilization in translucent material part is covered thereto in the transparent material or article production process
Template spraying is formed in step containing the centrical Nano diamond powder of nitrogen-sky or solution or other modes in translucent material
The specific pattern generated in rapid one.
Step 3：By the position containing marker graphic in the laser irradiation of the 532nm transparent material or article, and benefit
The optical signal for receiving sample reflection with filter plate, optical signal collection system and generating, obtains clearly fluorescent image after processing.
Step 4：By handling the optical signal being collected into, the image of fluorescence signal is obtained.To this image, into
Row decoding (as scanned this pattern using mobile phone, just as two dimensional code, obtains information representated by pattern), then by with
The information comparison stored in server, can know whether as genuine piece.
Scheme two
The program two may include following steps：
Step 1：Article for certain type of transparent material composition or comprising a part of translucent material generates its spy
Different Nano diamond size, concentration information, at the same by the figure and it includes information store into server.
Step 2：In the transparent material or article production process during translucent material part producing thereto according to
The concentration ratio addition Nano diamond powder or solution determined in step 1, formation contain the transparent of fluorescence nano diamond
Material；Object further can be assembled by the transparent material for containing fluorescence nano diamond for the article comprising translucent material
On product.
Step 3：Pass through the position containing fluorescence nano diamond in the laser irradiation of the 532nm transparent material or article
The optical signal for setting, and receiving sample reflection using filter plate, optical signal collection system and generating, obtains clearly glimmering after processing
Light image.
Step 4：By handling the optical signal being collected into, the image of fluorescence signal is obtained.To this image into
Row concentration and Nano diamond dimension analysis, then by comparing with the information stored in server, can know whether to be true
Product.
Embodiment 3
By using containing the centrical Nano diamond of nitrogen-sky realize solution it is anti-fake may include following steps：
Step 1：For certain specific solution, its special Nano diamond size and concentration (this size are designed
And concentration information can be with the title of corresponding solution, formula, effect etc. information), at the same by the concentration and it includes information deposit
It stores up in server.
Step 2：The Nano diamond of specific dimensions, quality is added into solution during solution bottling, encapsulation
Powder (or Nano diamond solution of certain concentration and volume).
Step 3：It takes solution to be measured that sample is made, is irradiated under the laser of 532nm, and collect system using filter plate and light
System obtains the optical signal of electromagnetic radiation, reflection.
Step 4：By the optical signal prosessing to acquisition, the size and concentration of Nano diamond in the sample are obtained, with
The information comparison stored in server, can know whether as genuine piece.
Embodiment 4
Take Prussian blue logical ink 10mL as sample A, the Nano diamond for taking common blue ink 10mL that 10 μ L are added is water-soluble
Liquid sufficiently vibrates, and ultrasound 10 minutes, is denoted as sample B.Nano diamond solution weight percentage used is 0.1wt%, is received
Rice diamond partial size is about 50nm.
By sample A, B ultrapure water by volume 1：5 to be diluted to color more transparent, drips on glass slide, dries water
Point.
In specific detection, it can use homemade laser scanning co-focusing microscope and two glass slides applied respectively
The laser of 532nm is simultaneously observed, and can be found fluorescence signal in sample B, can be told truth from falsehood.
In specific application, anti-counterfeiting ink can be scribbled to the surface of the article of pending anti-fake processing, utilizes the anti-fake ink
The fluorescence that Nano diamond particle contained by water is issued in the case where wavelength is the excitation of 532nm, carries out anti-fake.
Embodiment 5
By realizing that paper false proof mainly includes following steps using containing the centrical Nano diamond of nitrogen-sky：
Different paper is designed different safety drawings (two dimensional code, bar code or other figures), and is stored into database, by this
Mask is made in kind safety drawing, sprays Nano diamond solution using mask in paper specific region.
When detecting, paper can be irradiated under the laser of 532nm, and obtains sample using filter plate and light collecting system
The optical signal of product transmitting, reflection.By the optical signal prosessing to acquisition, the safety drawing of sample surfaces is obtained, in database
Thus data comparison judges whether paper is genuine piece.
Other than the light of 532nm wavelength applied in above-described embodiment, the present invention can also use 400nm to 600nm
Laser, NV Nano diamond can inspire fluorescence by the laser of 400nm to 600nm.Judgement for fluorescence, this
Invention collects the light that NV diamond generates preferably using 600nm as line of demarcation, using equipment, by filter plate by 600nm or less
Light filter and (also avoid that laser will be inputted in this way, if the input laser of 532nm is as fluorescence signal collection).For example, filtering
Single photon counting module can be passed through behind wave plate[30]Optical signal is collected, point of the number of photons greater than 600nm wavelength is obtained
Cloth information, if there is be collected into be greater than 600nm light can think there is fluorescence signal.In addition, as shown in Figure 2 and Figure 3, due to
The optical wavelength that NV diamond issues, between 800nm, other than 600nm, can also use other wavelength value conducts in 550nm
Critical value.
Nano diamond particle employed in above-described embodiment, partial size are 5nm~500nm, and contained by inside
NV-Concentration meets 10ppm to 100ppm.At present in the Nano diamond of commercial sale nitrogen impurity concentration be 100~
200ppm, and NV is converted by these nitrogen-Conversion ratio generally only has 10% or so, that is, the Nano diamond of general commercial sale
Its NV-Concentration is generally 10ppm, and concentration is not especially big, it is contemplated that increases the NV in single Nano diamond-Concentration can mention
High fluorescent can increase the NV in single Nano diamond as far as possible-Concentration, to increase the accuracy of detection, such as
Nano diamond can be produced using artificial means (such as by the way of ion implanting), by NV-100ppm or so is arrived in concentration promotion.
Edible glue in the present invention can be using any one edible glue in the prior art.It is of the present invention containing
Nitrogen-vacancy center NV- Nano diamond can be used commercial sources and buy, naturally it is also possible to (e.g., with reference to related art
Preparation, coherence and temperature sensing research [D] the China Science & Technology University of Wang Junfeng diamond NV colour center, 2016.) from
Row preparation.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all wrap
Containing within protection scope of the present invention.
Claims (10)
1. a kind of method for anti-counterfeit based on Nano diamond, which is characterized in that this method is by pending anti-fake processing
The surface coated with nano diamond particles of article, or by mixing nanometer Buddha's warrior attendant inside the article to pending anti-fake processing
Nitrogen-vacancy center NV in negative charge state is contained in stone particle, these Nano diamond particles inside-, utilize these nanogold
The fluorescence that hard rock particle is issued in the case where wavelength is the excitation of 400nm~600nm, carries out anti-fake；Preferably, these nanometers
The partial size of diamond particles is 5nm~500nm, NV contained by inside-Concentration control is 10ppm to 100ppm.
2. as described in claim 1 based on the method for anti-counterfeit of Nano diamond, which is characterized in that when detecting, be by to
The surface or article to be detected for detecting article or article to be detected crush composition granule or solute is article crushed material to be detected
Apply the exciting light that wavelength is 400nm~600nm in the solution of grain, then by detecting whether to inspire fluorescence, carries out anti-fake；
When not detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is fakement；
When detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is genuine piece.
3. as claimed in claim 2 based on the method for anti-counterfeit of Nano diamond, which is characterized in that the Detection wavelength of the fluorescence is excellent
Choosing is greater than 600nm；
Preferably, the wavelength of the exciting light be 532nm, the Detection wavelength of the fluorescence be preferably greater than 600nm and be less than etc.
In 800nm.
4. as described in claim 1 based on the method for anti-counterfeit of Nano diamond, which is characterized in that the pending anti-fake processing
Article is drug.
5. a kind of drug anti-fake based on Nano diamond, which is characterized in that be coated with Nano diamond on the surface of the drug
Particle, or in the inside of the drug include Nano diamond particle, the inside of these Nano diamond particles is contained in negative
The nitrogen of state of charge-vacancy center NV-, for issuing fluorescence under the excitation for the exciting light that wavelength is 400nm~600nm, into
Row is anti-fake；Preferably, the partial size of these Nano diamond particles is 5nm~500nm, NV contained by inside-Concentration controls
10ppm to 100ppm.
6. the drug anti-fake based on Nano diamond as claimed in claim 5, which is characterized in that the Nano diamond particle is logical
Cross the surface that edible glue is coated in the drug；Preferably, the Nano diamond particle is in the form of the pattern being pre-designed
Or the pattern of random distribution formation is arranged in the surface of the drug, the pattern being pre-designed is more preferably bar code pattern
Or pattern in 2 D code, the bar code pattern or pattern in 2 D code are for associated with the information of tracing to the source of the drug.
7. a kind of anti-counterfeiting ink based on Nano diamond, which is characterized in that the anti-counterfeiting ink includes Nano diamond particle,
Contain the nitrogen in negative charge state-vacancy center NV in the inside of these Nano diamond particles-, for wavelength be 400nm~
Fluorescence is issued under the excitation of the exciting light of 600nm, is carried out anti-fake；Preferably, the partial size of these Nano diamond particles be 5nm~
500nm, inside contained by NV-Concentration control is 10ppm to 100ppm.
8. as claimed in claim 7 based on the anti-counterfeiting ink of Nano diamond, which is characterized in that the wavelength of the fluorescence is
550nm~800nm, preferably greater than 600nm and be less than or equal to 800nm；
Preferably, the wavelength of the exciting light is 532nm.
9. the application as described in claim 7 or 8 based on the anti-counterfeiting ink of Nano diamond in anti-fake.
10. application as claimed in claim 9, which is characterized in that the application is specifically to the article of pending anti-fake processing
Anti-counterfeiting ink is scribbled on surface, using Nano diamond particle contained by the anti-counterfeiting ink in the excitation that wavelength is 400nm~600nm
The lower fluorescence issued of light excitation, carries out anti-fake；
Preferably, when detecting, by applying the exciting light that wavelength is 400nm~600nm on the surface of article to be detected, so
Afterwards by detecting whether to inspire fluorescence, carry out anti-fake；
When not detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is fakement；
When detecting wavelength is the fluorescence of 550nm~800nm, then the article to be detected is genuine piece.
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Application publication date: 20181130 |