Carbide-silicon nitride luminophores

FIELD: physics.

SUBSTANCE: luminophore consists of crystal lattice of seed material with activating additives representing ions Eu2+, Tb3+ and/or Eu3+. Said seed material, when excited by high-energy excitation radiation, absorbs at least portion of said excitation radiation to, then, emit radiation with lower power. Note here that seed material lattice represents carbide-silicon nitride compounds not containing cerium as activating additive. Invention covers also luminophore with its seed material lattice represents compound with general formula Ln2Si4N6C, where Ln stands for element or mix of elements selected from group including yttrium, lanthanum, gadolinium and lutetium.

EFFECT: reduced tendency to luminescence quenching, higher temperature and chemical stability.

11 cl, 6 dwg, 4 ex


The invention relates to inorganic luminescense materials that can absorb excitation radiation of high energy and high efficiency to turn it into emitted radiation at a lower energy. At the same time as the excitation radiation may use especially ultraviolet radiation or blue light, from which the conversion process receive radiation in the green, yellow, orange and/or red region of the visible spectrum.

It has long been known that inorganic phosphors will be used to render images in an invisible radiation (e.g. x-rays or in the manufacture of screens), and in General for lighting (e.g. fluorescent lamps or in the manufacture of LEDs). Such phosphors typically have a crystalline lattice of the seed material, which is introduced additives special elements. By using technique as a lattice of the seed material such phosphors are still used mainly sulfides, halides and oxides or, in a particularly great extent, complex salts of oxygen-containing acids (borates, aluminates, silicates, phosphates, molybdates, wolframates etc).

Only in recent years has been to learn as lattices crystal core for the synthesis of the EF is an objective of the phosphors and nitride ( for example, described Hintzen et al. in the European patents EP 1104799 A1 and EP 1238041 B1 connection type M2Si5N8:Eu2+where M=CA, Sr, Ba, with a red light) and oxynitride substances (as an example, you should call connection MSi2O2N2according to Delsing et al. in the international application WO 2004/030109 A1; M=CA, Sr, Ba, and blue, green and yellow light). Interest in such phosphors have since increased significantly primarily due to the feasibility of their use as phosphors converters in the manufacture of white LEDs. This is due primarily to the fact that, as expected, the materials of this type due to the high of bond Covalence of chemical bonds and confirmed a pronounced stiffness of the main grid have very high chemical and thermal stability. Disadvantages most of sulfide phosphors converters and those dominated by oxygen consist primarily in the fact that the yield of luminescence, usually very quickly drops when the temperature exceeds 100°C. For production of advanced white LEDs with a higher power that is required, however, phosphors-converters with a much better temperature stability.

On the other hand, in this regard, it should be noted that in the e without exception, are now used in the technique of inorganic phosphors-converters (yttrium aluminate, thiogallate, sulfides and silicates of alkaline earth metals, nitrides, oxynitrides), which are used to produce white light in combination with led blue light is activated Eu2+or CE3+with an extremely broad band emission. For such phosphors characteristic electronic transitions 5d-4f, which are exposed to the external field in the crystal and, thus, of course, also centers extinguish, if any. Accordingly, the situation is fundamentally different from that of the application of the phosphors in fluorescent lamps. In this case, as the green and red component mainly use phosphors with bar specturm emission, the luminescence of which is based on transitions between the 4f-electrons (transitions of 4f-4f), a well-shielded from external fields crystals.

A high proportion of covalent bonds is characteristic also for another class of compounds, discovered only recently. We are talking about SIC-nitrilotriacetic containing rare earth or alkaline earth metals. Managed to synthesize and characterize from the point of view of the basic physico-chemical properties of the first substances are representatives of this class of materials (for example, the compounds of Ho2Si4N6C, Tb2Si4N6C (see Nørre et al. J.Mater. Chem 11 (2001) 3300) and (La,Y,Ca)2(i,Al) 4(N,C)7(see Liddel et al. J. Eur. Ceram Soc. 25 (2005) 37).

In the professional literature is still absolutely no information about the luminescence of these compounds. Now, however, Schmidt et al. presented in the international application WO 2005/083037 A1, published after the priority date of this application, carbide-nitriloacetate material activated by cerium, in particular, the phosphors of the Y2Si4N6C:Ce with the concentration of the activator component 5% CE. These materials lumines cent in the broad area of the yellow part of the spectrum when excited by ultraviolet radiation or light of a blue led and, according to published data, in aspects of quantum yield, absorption efficiency and thermal performance have properties indistinguishable from those of the other well-known phosphors converters with yellow light, as, for example, yttrium aluminum garnet, also with the addition of cerium or orthosilicates alkaline earth metals with activation of Eu2+.

The present invention, in contrast, is to offer new carbide-nitriloacetate phosphors, in particular, for use in white LEDs high power, different primary or improved characteristics of luminescence.

This problem is solved phosphors determined the military in claims 1 and 2.

The materials according to the invention belong to the class of turbidometric, in particular SIC-nitrilotriacetic. They can be used as phosphors converters, in pure form or in mixture with other appropriate phosphors, for the manufacture of light sources, in particular for the production of LEDs with white light.

Introduction to appropriate nitrilotriethanol matrix ions is associated with increasing covalently lattice. Taking into account this fact as a special advantage of the phosphors according to the invention, mention should be made, for example, reduced susceptibility to thermal quenching of luminescence, high chemical and thermal stability and low tendency to aging.

The General formula of the basic lattice of the phosphors according to the invention is as follows:


where 0≤a≤2, 0≤b < 1, 0≤c<4, 0≤d<4, 0≤e<1, 0≤f≤(a+b) and 0≤(b+e)<1, and Ln denotes at least one metal from the group including indium (In), scandium (Sc), yttrium (Y) and rare earth elements, in particular elements lanthanum (La), gadolinium (Gd) and lutetium (Lu) or a mixture of these metals.

As indicated in the General formula, a special form of execution of the Ln may also be fully or partially replaced dohale tym metal M Ipreferably zinc (Zn) or alkaline earth metals such as magnesium (Mg), calcium (CA), strontium (Sr) and barium (BA), if at the same time equimolar amount of nitrogen (N) substituted by oxygen (O) or carbon (C) nitrogen (N).

In another modified form of execution is also possible substitution of silicon (Si) component of MIIsuch as germanium (Ge), and/or boron (B), and/or aluminum (Al). In the latter cases it is also necessary the substitution of equimolar amounts of N-oxygen, carbon-nitrogen N, or metal MImetal Ln.

Depending on the exact composition of the main lattice of the phosphor, the formation of different crystal structures with different points of embedding activator ions of rare earth and/or transition metals. Preferred activators are cerium and/or terbium and europium or certain elements are transition metals, which can be embedded in a matrix in the form of divalent (especially Eu2+) or trivalent (in particular, CE3+, Tb3+, Eu3+) ions.

The concentration of the activator can comprise from 0.001 to 1.5 moles of activator per mole of phosphor. Cerium, optionally added as activator may be present in concentrations from 0.0005 to 1.5 mol of cerium per mole of phosphor.

A preferred form filled with what I phosphors according to the invention is defined by the following formulas:



or Ln(2-x)Si4N6C:Eux,

in each case Ln=Y, La, Gd and/or Lu and of 0.001<x<1.0, and also of 0.001≤y≤1,0.

The phosphors according to the invention when excited in the UV (200-380 nm) or violet (380-420 nm) or blue (420-480 nm) spectral region emit green, yellow, orange or red fluorescent radiation. They are characterized by high absorption of the exciting radiation, and in addition, have a high quantum yield and low temperature quenching of the luminescence.

Due to these characteristics and other desirable properties of the phosphors according to the invention it is expedient to apply either as separate components or as a mixture of several phosphors according to the invention or combined (mixed) with other well-known phosphors-converters with the emission of blue, green, yellow or red for the manufacture of white LEDs.

The present invention is the first efficient phosphors for manufacturing white LEDs with linear spectra of 4f-4f excited in the blue region of the spectrum, activated rare earth elements. Unexpectedly proved that the simultaneous introduction with signs image is the shadow the basic crystal lattice of SIC-nitrilotriacetic phosphors ions of terbium and cerium leads to the green line emission Tb 3+excited by light of a blue led. Phosphors activated by rare earth elements, with linear spectra of 4f-4f have already mentioned advantages in terms of resistance to external fields crystals and external factors extinguishing. In addition, when using carbonitridation phosphors according to the invention, with joint supplements CE3+and Tb3+as the green component of the white led can take advantage of other benefits. Firstly, the main peak of emission of Tb3+located at a wavelength of about 545 nm, characterized by extremely small width compared to the broadband spectra, secondly, the emission spectrum consists of other groups of lines distributed throughout the visible region of the spectrum. The property, called the first, favorably when using white LEDs for background lighting of LCD screens (coordination characteristics of the radiation used by the filter), while the typical (within certain limits by varying the ratio CE/Tb) controlled spectral distribution of the luminescence of phosphors, jointly activated CE3+-Tb3+helps improve color output values CRI) for use in white light the diodes for General lighting.

Another important advantage of the present inventive solution is the fact that with its help it is possible to synthesize a new phosphor Converter with a red glow. In inorganic nitride compounds can provide a much stronger field of crystals than in the case of phosphors is dominated by oxygen. This is an important prerequisite for the desired red shift of the luminescence emitted by, for example, ions of Eu2+.

Experiments conducted in connection with the present invention, unexpectedly showed that the phosphors with red emission with excitation spectrum, suitable for use in white LEDs, can also be obtained when the additive into the main grid according to the invention europium ions.

Other details, advantages and forms of execution of the present invention are clear from the description of the conditions of synthesis of phosphors, as well as from the accompanying drawings, which depict:

Figure 1 spectra of excitation (left side of illustration) and emission (right side) of the phosphor Y2Si4N6C with the addition of cerium,

Figure 2 - spectrum of the diffuse reflection, excitation spectrum and linear spectrum of emission of Y2Si4N6C-phosphorus-activated Tb3+,

Figure 3 - excitation spectrum (left side of illustration) and emission (right side) Y2S 4N6C-material joint addition of CE and Tb,

Figure 4 - range of excitation and emission of the phosphor, activated by europium.

Synthesis containing rare earth or alkaline earth metals SIC-nitrilotriacetic described above General formula, it is advisable to carry out the method of reaction in the solid phase at high temperature. The synthesis process is described below as an example of the General preparative sample, and also by means of two examples of execution carbonitridation phosphors with the addition of CE and Tb or Eu.

As initial components using α-Si3N4, β-Si3N4, coal powder, SiC, and rare earth elements yttrium, cerium, terbium and europium, in each case in the metallic form. Before proceeding to the subsequent stages of the process rare earths first attirbute in the atmosphere of nitrogen or ammonia. Then nitrated compounds added to Si3N4, SiC or coal powder in the appropriate stoichiometric ratios, when the required number, and intensively stirred. Because some components are hygroscopic, all these manipulations should be carried out in glove the camera in a dry nitrogen atmosphere. The powder mixture is placed in the crucibles of the appropriate size and calcined at high temperature furnace at temperature the round from 1500 to 1800°C. for 2-48 hours in an atmosphere of pure nitrogen. After the process of annealing the samples cooled to room temperature and, if necessary, subjected to further appropriate treatment.

Example 1

To prepare activated by terbium and cerium carbide-nitriloacetate Y1,00Si4N6C:Tb0,99Ce0,01metal terbium first attirbute at 1200°C for 12 hours in a horizontal tube furnace in an atmosphere of pure nitrogen to TbNx(x≈0,99).

Educt - 34,24 g TbNx; 17,78 g of metallic yttrium; 0.28 g of metallic cerium; 28,06 g of α-Si3N4and 8,02 g SiC, then intensively mixed in an agate mortar in a dry nitrogen atmosphere and placed in a molybdenum crucible. This powder mixture cast in an atmosphere of pure nitrogen for 10 hours at 1600°C, and then in the same furnace cooled to room temperature. After removal of unreacted and soluble components receive the phosphor with the green glow of the Y1,00Si4N6C:Tb0,99Ce0,01.

Example 2

For the production of activated 5% europium SIC-nitrilotriacetic composition Gda 1.8Srof 0.2Si4N6,2C0,8pure metal strontium and europium attirbute at 850°C for two hours in a horizontal tube furnace in an atmosphere of pure nitrogen to predecessors Sr3N2and EuN. Then 56,61 g meta is symbolic of gadolinium; only 2.91 g Sr3N2; 1.66 g EuN; 29,93 g of α-Si3N4and 6.42 per g of SiC thoroughly mixed in a dry nitrogen atmosphere and placed in a heat-resistant crucible. The calcination of the mixture is carried out for 24 hours at 1750°C in a nitrogen-hydrogen atmosphere (90:10). After proper subsequent processing of the sample receive a phosphor with a strong red luminescence.

Additional examples of SIC-nitrilotriacetic phosphors

Example 3

To prepare activated with terbium SIC-nitriloacetate composition Lu1,6Tbfor 0.4Si4N6C metal terbium first nitrous as described in example 1 description of the invention, TbNx(x≈0,99). Then 6,912 g powder TbNx, 28,00 g of powder metal lutetium, 18,70 g of α-Si3N4and 1,201 g of graphite powder (carbon powder) in a dry nitrogen atmosphere intensively mixed in an agate mortar and loaded into a molybdenum crucible. The powder mixture is calcined in an atmosphere of pure nitrogen at a temperature of 1700°C for 20 h and then leave to cool in the furnace. Get a phosphor emitting green light (figure 5).

Example 4

To prepare activated by cerium and terbium SIC-nitriloacetate composition of La0,99Ce0,01TbSi4N6C in a sealed box with gloves weighed under the atmosphere of dry nitrogen 23,84 g metal Terb what I 20,63 g of a powder of metallic lanthanum, 0,210 g of metal powder of cerium, 21,04 g of α-Si3N4and 6,014 g of silicon carbide and intensively mixed in an agate mortar. The powder mixture is placed in a molybdenum crucible with lid, is subjected to firing in an atmosphere of pure nitrogen at a temperature of 1650°C for 10 h and then leave to cool in the furnace. Get a phosphor emitting blue-green emission when excited by radiation with a wavelength of 370 nm, which is characterized by a typical activated by terbium phosphors spectrum in the green region of wavelengths (Fig.6).

The accompanying drawings fully clear to the expert in the phosphors and are self-explanatory. Basic data about the present state of things were mentioned above. Below in the order of additions was given instructions on some features.

From Figure 1 it is seen that all the phosphors Y2Si4N6C with the addition of cerium lumines cent in the yellow-green region of the spectrum upon excitation between 360 and 450 nm. Different curves in each case refer to different concentrations of additives, the magnitude of which is also shown on the chart.

Figure 2 shows that the activated Tb3+phosphors Y2Si4N6C you must initiate in the region from 280 to 320 nm, in order to obtain an effective bar green emission of Tb3+.

From Figure 3 it is clearly seen, is the root lattice of Y 2Si4N6C with the joint addition of CE and Tb is also possible to excite between 360 and 450 nm. In the selected example, it ruled emission of Tb3+overlaid with broadband emission of CE. You can, however, find the ratio of the concentrations of CE/Tb, which ruled emission of terbium has a significant superiority and luminescence of cerium strongly suppressed.

Finally, from Figure 4 it is clear that the bandwidth of the emission matrix, activated by europium, registered at the maximum wavelength of 610 nm, can also be obtained upon excitation in the range between 350 and 480 nm.

Although the details were described only certain forms of execution, the specialist it is clear that there are many options phosphor according to the invention. The possibility of variation was demonstrated by General formulas and naming possible elements of the successor.

1. The phosphor for use in white light sources with high power, consisting of the crystal lattice of the seed material with additives-activators, which represents ions of Eu2+, Tb3+and/or Eu3+that upon excitation of its high-energy radiation excitation absorbs at least part of this exciting radiation and then emits radiation with ENISA energy characterized in that the lattice of the seed material is carbamodithioato compound which does not contain additives of cerium as an activator.

2. A phosphor comprising a crystal lattice of the seed material with additives-activators, which represents ions of Eu2+CE3+, Tb3+and/or Eu3+that upon excitation of its high-energy radiation excitation absorbs at least part of this exciting radiation and then emits radiation of lower energy, characterized in that the lattice of the seed material is a compound with the following General formula:
and Ln means the element or mixture of elements selected from the group comprising yttrium, lanthanum, gadolinium and lutetium.

3. The phosphor according to claim 2, characterized in that the crystal lattice of the seed material as activators added ions Tb3+and as coactivators ions CE3+.

4. The phosphor according to claim 2, characterized in that the concentration of the activator is from 0.001 to 1.5 moles of activator per mole of phosphor.

5. The phosphor according to claim 3, characterized in that as coactivator in the crystal lattice of the seed material added cerium in a concentration of from 0.0005 to 1.5 mol of cerium per mole of phosphor.

6. The phosphor according to claim 1, characterized in that it is defined by one of the following General formula:
in each case Ln=Y, La, Gd and/or Lu and of 0.001<x<1.5, and also of 0.0005≤y≤1,5.

7. The phosphor according to one of claims 1 to 6, characterized in that when the excitation radiation with wavelengths 200-480 nm, it emits green, yellow, orange or red radiation.

8. The phosphor according to claim 1, characterized in that upon excitation with blue light it emits radiation with a linear spectrum is due to electronic transitions of 4f-4f.

9. A white light source, characterized in that it includes a light-emitting element and at least one phosphor according to one of claims 1 to 8, excited by radiation generated emitting element, and emits green, yellow or red radiation.

10. The light source according to claim 9, characterized in that the light-emitting element is an led.

11. The light source of claim 10, wherein the led emits in the wavelength range 200-480 nm.


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FIELD: physics.

SUBSTANCE: described is light-converting material containing a matrix and at least one composite which converts UV radiation to radiation of a different colour, with particle size from 10 nm to 1000 nm, selected from a group ZnO:Zn and rare-earth element compounds of formula: MexaAybRzc , where Me denotes a metal, selected from a group comprising yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, ytterbium, aluminium, bismuth, manganese, calcium, strontium, barium, zinc or mixture thereof; A denotes a metal selected from a group comprising cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, terbium, ytterbium, titanium, manganese; R is an element selected from a group comprising oxygen, sulphur, boron, titanium, aluminium and/or compounds thereof with each other; a, b and c denote the charge on the Me ion, A or R, respectively, x≥1, 1.0 ≥ y ≥ 0.0001, z is defined by ax + by = cz. The invention also describes a composition for producing said material, containing the following in wt %: said composite - 0.001-10.0; matrix-forming component - the rest.

EFFECT: invention increases intensity of converting UV radiation to infrared radiation, blue to green spectrum region, and therefore increases plant yield.

27 cl, 25 ex

FIELD: chemistry.

SUBSTANCE: invention can be used in production of inorganic yttrium oxysulphide-based multifunctional anti-Stokes luminophors which can be used for converting infrared radiation to visible luminescence, for protecting bond paper and documents, strict accounting forms, conformity marks of goods and articles, excise and identification marks, banknotes, as well as for making emergency and signal light systems, evacuation, fire, warning and indicator light marks, for pointers in shafts, tunnels, overpasses, metro and passages for information-direction boards in motorways and decorative cosmetics. The yttrium oxysulphide-based luminophor is activated by titanium ions and coactivated by magnesium ions, and also contains a cationic sublattice of trivalent ytterbium and erbium ions and has a chemical composition corresponding to the following empirical formula: (Y1-X-YYbxEry)202S:Ti0.12,Mg0.04, where 0.01<X<0.05; 0.01<Y<0.05.

EFFECT: more intense visible anti-Stokes luminescence during excitation of infrared radiation in the 0,90-0,98 mcm range.

7 cl, 1 tbl, 4 dwg

FIELD: chemistry.

SUBSTANCE: invention describes a method of modifying anti-Stokes luminophors based on oxychlorides of rare-earth elements, involving treatment of a luminophor with low-melting glass with flow temperature of 560-600°C in amount of 7-20% of the weight of the initial luminophor at 560-600°C for 0.5-1 hour.

EFFECT: obtaining modified anti-Stokes luminophor with high output and high moisture resistance with retention of high level of luminous intensity during infrared excitation.

9 ex