CN103108843A - Fluorine-containing magnesium oxide light-emitting body and method for producing same - Google Patents

Fluorine-containing magnesium oxide light-emitting body and method for producing same Download PDF

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Publication number
CN103108843A
CN103108843A CN2011800463597A CN201180046359A CN103108843A CN 103108843 A CN103108843 A CN 103108843A CN 2011800463597 A CN2011800463597 A CN 2011800463597A CN 201180046359 A CN201180046359 A CN 201180046359A CN 103108843 A CN103108843 A CN 103108843A
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fluorine
magnesium oxide
twinkler
magnesium
light
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CN2011800463597A
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CN103108843B (en
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大崎善久
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Tateho Chemical Industries Co Ltd
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Tateho Chemical Industries Co Ltd
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/12—Light sources with substantially two-dimensional radiating surfaces
    • H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source
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    • C09K11/55—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing beryllium, magnesium, alkali metals or alkaline earth metals
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    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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    • C01F5/00—Compounds of magnesium
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Abstract

Provided is a fluorine-containing magnesium oxide light-emitting body having an ultraviolet light emission strength that is at least at the level of that of magnesium oxide containing more than 100 ppm of fluorine, despite containing less than 100 ppm of fluorine. The magnesium oxide light-emitting body has a light-emission peak in the ultraviolet region of 200-300 nm on the basis of excitation by an electron beam or ultraviolet rays, has an amount of contained fluorine with respect to magnesium of less than 100 ppm, and has a light-emission peak strength ratio with respect to the reflection peak (wavelength around 980 nm) of the excitation-light lamp of at least 20. The light-emitting body can be obtained by adding to a magnesium oxide precursor a fluorine compound at an amount resulting in 0.06-1.25 mol% of fluorine with respect to magnesium, firing, temporarily cooling, and then reheating.

Description

Fluorine-containing magnesium oxide twinkler and manufacture method thereof
Technical field
The present invention relates to fluorine-containing magnesium oxide twinkler and manufacture method thereof.
Background technology
Plasma panel (Plasma Display Panel; PDP) be the display equipment that utilizes the emissive type of discharge, owing to can show image bright-coloured and that video resolution is high, and than being easier to realize large picture, so be widely used as large-sized panel display device.
In the discharge space of AC plasma display screen (AC type PDP), by the surface at dielectric layer, protective layer is set, reduce operating voltage, and protect dielectric layer in the plasma body that produces in discharge space.In the past, the magnesium oxide of high, the anti-sputtering excellence of secondary electron yield was widely used as the material that is used to form this protective layer.
In addition; take the discharge characteristic that improves AC type PDP and the characteristics of luminescence etc. as purpose; propose the UV-light (vacuum-ultraviolet light) that the surface configuration in the discharge space side of described protective layer produced by the geseous discharge by Xe gas and excited, and discharged the scheme of the material of UV-light.In patent documentation 1, near the fluorine-containing magnesium oxide powder that has the glow peak of UV-light wavelength 250nm is disclosed as such material.Near the release of the UV-light this wavelength 250nm plays a role to the improvement of the luminous efficiency of AC type PDP.
But, the fluorine content of only having put down in writing in patent documentation 1 in fluorine-containing magnesium oxide powder is defined as 0.01 % by weight, is (claim 1) more than 100ppm, in an embodiment, fluorine content is that magnesium oxide more than 100ppm is in a ratio of (table 2 and paragraph [0032]) below 1/10th less than the UV-light luminous intensity shown in the magnesium oxide of 100ppm and fluorine content.Again, having put down in writing this fluorine-containing magnesian manufacture method is to burn till magnesium oxide powder (paragraph [0019]) under the existence in fluorine source.
Put down in writing similarly to be provided with by the triggering particle that consists of more than adding 24ppm, less than the magnesium oxide xln of the halogen elements such as fluorine of 100ppm at the dielectric layer of PDP and protective layer in patent documentation 2 and emitted layer (claim 1 and a claim 2) again.Wherein put down in writing this triggering particle and emitted layer and improve discharge delay by discharge triggering particle to discharge space, and put down in writing to the interpolation of the fluorine of magnesium oxide xln and the relation between discharge delay.But, about emit by this triggering particle the layer UV-light luminous without the record.In the document, as fluorine-containing magnesian manufacture method, also just put down in writing mixed oxidization magnesium xln and contained the material of halogen and the content of burning till (paragraph [0024]) again.
Although not relevant to fluorine-containing magnesium oxide, put down in writing the content (claim 1) in the fluorophor particle surface formation fluorine-containing coat of PDP in patent documentation 3.When wherein having put down in writing the fluorine containing ratio in improving described coating, more fluorine is discharged in the PDP discharge space, thereby can make the discharge ionization voltage rising (paragraph [0059]) of PDP.
The prior art document:
Patent documentation:
Patent documentation 1: TOHKEMY 2007-254269 communique;
Patent documentation 2: No. 4492638 specification sheets of Japan's special permission;
Patent documentation 3: TOHKEMY 2005-100954 communique.
Summary of the invention
The problem that invention will solve:
When thinking fluorine amount in reduction is discharged into discharge space by the record content of patent documentation 3, the discharge ionization voltage of PDP can descend.Therefore, it is desirable to reduce in the material of the UV-light releasing layer in being disposed at the PDP discharge space fluorine content.But according to the record of patent documentation 1, the fluorine content in fluorine-containing magnesium oxide powder is during less than 100ppm, and the UV-light burst size can descend, and therefore can not expect the effect as the UV-light releasable material.
The present invention is in view of above-mentioned present situation, no matter the problem that will solve is to provide fluorine content less than 100ppm, and has and the fluorine-containing magnesium oxide twinkler that contains greater than the UV-light luminous intensity more than the magnesium oxide equal extent of the fluorine of 100ppm.
The means of dealing with problems:
The inventor etc. are in order to address the above problem the result that repeats various discussions, found to utilize specific method to make fluorine-containing magnesium oxide twinkler, no matter less than 100ppm, and can access the magnesium oxide twinkler that sends UV-light with the intensity of abundance with this fluorine content, thereby complete the present invention.
Namely the present invention relates to fluorine-containing magnesium oxide twinkler, be based on by electron beam or the UV-induced magnesium oxide twinkler that has glow peak in 200～300nm ultra-violet region that excites, wherein, less than 100ppm, and the strength ratio that described glow peak is near the reflection peak of the laser lamp 980nm with respect to wavelength is more than 20 with respect to magnesian fluorine content.
It is desirable in described twinkler the metallic element of 1 valency more than containing 50ppm with respect to magnesium oxide, less than 300ppm, divalent, 3 valencys or 4 valencys (still, beyond demagging).
It is desirable in described twinkler, described metallic element is one or more that select from the group who is comprised of Li, Be, Na, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sb, Sn, Cs, Ba, Hf, Ta, Ir, Au, Tl, Pb, Bi, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
In described twinkler, preferably with the magnesian purity calculated except fluorine or in the situation that comprise described metallic element, be more than 99.9 quality % with the magnesian purity of calculating except fluorine and metallic element.
Described twinkler is preferably the accumulation 50% particle diameter (D by the volume reference of passing through laser diffraction and scattering formula particle size distribution 50) be that the fluorine-containing magnesium oxide powder that 0.8 μ m is above, 4.0 μ m are following forms.
Described twinkler is preferably used for being configured in the discharge space of plasma panel.
Again, the present invention relates to make the method for described twinkler, comprise: in the magnesium oxide precursor, add fluorine cpd and burn till with respect to the amount that magnesium reaches 0.06～1.25mol% with fluorine, obtaining fluorine-containing magnesian operation with this; After temporary transient cooling described fluorine-containing magnesium oxide, by again being fired into the operation of described twinkler.
Described magnesium oxide precursor is preferably selected from the group who is comprised of magnesium hydroxide, alkaline magnesium carbonate, magnesiumcarbonate, magnesium acetate, magnesium nitrate and magnesium oxalate.
The effect of invention:
No matter magnesium oxide twinkler fluorine content of the present invention less than 100ppm, has and contains greater than the UV-light luminous intensity more than the magnesium oxide equal extent of the fluorine of 100ppm.By magnesium oxide twinkler of the present invention is configured in the discharge space of PDP, can increase the burst size of the UV-light in discharge space, can increase the light quantity of the visible light that sends from gas discharge luminescent device.Again, when the burst size of general UV-light was more, the release that triggers particle also increased, and therefore magnesium oxide twinkler of the present invention can improve the discharge delay in PDP.Therefore, magnesium oxide twinkler of the present invention can be fit to use as the lip-deep UV-light releasing layer of the discharge space side of the dielectric material protective layer that is formed at AC type PDP.
In addition, the fluorine content of magnesium oxide twinkler of the present invention is less than 100ppm, and the fluorine amount that therefore is discharged in discharge space descends, thereby can suppress the rising of the discharge ionization voltage of PDP.
Embodiment
At first, twinkler of the present invention is described.
Twinkler of the present invention is formed by fluorine-containing magnesium oxide.Twinkler of the present invention forms as main body with highly purified magnesium oxide, more than magnesian purity (do not comprise fluorine content and calculate purity) is preferably 99.9 quality %.
In twinkler of the present invention, fluorine is included in magnesium oxide with the additive form.Be less than 100ppm with respect to magnesian fluorine content.When fluorine content surpassed 100ppm, the discharge ionization voltage of PDP may rise.Again, in the time fluorine content being reached burn till more than 5ppm, can avoid the particle growth in firing process, therefore more preferably 5ppm above, less than 100ppm.
The illuminated electron beam of twinkler of the present invention or when ultraviolet ray, realize having the luminous of glow peak in the ultra-violet region of wavelength 200～300nm based on exciting of causing thus.In addition, its luminous degree is that the strength ratio (glow peak/reflection peak) with respect near the above-mentioned glow peak of the reflection peak of the laser lamp wavelength 980nm is more than 20.When this peak intensity ratio is 20 when above, have and contain greater than the UV-light luminous intensity more than the magnesium oxide equal extent of the fluorine of 100ppm, therefore the raising of the luminous efficiency of PDP there is effect.By means of this, twinkler of the present invention be suitable as the dielectric material protective layer that is formed at AC type PDP the discharge space side lip-deep UV-light releasing layer and use.The strength ratio of above-mentioned glow peak is preferably more than 30.
Twinkler of the present invention is pulverous, and its particle diameter is preferably the accumulation 50% particle diameter (D by the volume reference of laser diffraction and scattering formula particle size distribution 50) be more than 0.8 μ m, below 4.0 μ m.Above-mentioned particle diameter is attempted to be coated on the surface of dielectric material protective layer less than the magnesium oxide powder of 0.8 μ m and when forming the UV-light releasing layer, due to easy cohesion, therefore be not easy to obtain good UV-light releasing layer.Again, when above-mentioned particle diameter surpasses 4.0 μ m, when on the surface that is configured in the dielectric material protective layer, the tendency that the optical transmission rate descends occurs.Above-mentioned particle diameter is that 0.8 μ m is above, 4.0 μ m are when following, and is dispersed better when being configured on the dielectric material protective layer by coating, again, and also without the problem that affects the optical transmission rate.Be preferably 1.0 μ m above, below 4.0 μ m, more preferably 1.5 μ m above, below 4.0 μ m.
The manufacture method of twinkler of the present invention then is described.
At first, (1) adds fluorine cpd in the magnesium oxide presoma.The temperature and time that burns till after considering and can suitably determine the addition of fluorine cpd, for example, fluorine is 0.06～1.25mol%, is preferably 0.1～1mol% with respect to the amount of magnesium.Excessive interpolation fluorine cpd in this stage, and after firing process in reduce fluorine content.
Above-mentioned magnesium oxide presoma refers to become magnesian compound by burning till.As the concrete kind of above-mentioned magnesium oxide presoma, such as enumerating magnesium hydroxide, alkaline magnesium carbonate, magnesiumcarbonate, magnesium acetate, magnesium nitrate, magnesium oxalate etc.Wherein, better because of the luminous intensity of resulting magnesium oxide twinkler, therefore be preferably magnesium hydroxide.
The magnesium oxide presoma is preferably the high presoma of purity, more than concrete purity is preferably 99.9 quality %, more preferably more than 99.95 quality %.
The modulator approach of above-mentioned magnesium oxide presoma is not particularly limited, but is preferably liquid-phase synthesis process.In order to utilize liquid-phase synthesis process modulation magnesium hydroxide, for example, the mixed chlorinated magnesium aqueous solution and aqueous sodium hydroxide solution obtain magnesium hydroxide slurry, and filter this slurries.The filter cake that filtration obtains is washed with deionized water, and in drying machine dry this filter cake, obtain magnesium hydroxide.
Described fluorine cpd are not particularly limited, but are preferably fluoride salt.Particularly, exemplify Potassium monofluoride, Sodium Fluoride, magnesium fluoride.For the magnesian purity that obtains is not descended, and be preferably magnesium fluoride.It is the above magnesium fluorides of 99.9 quality % that magnesium fluoride preferably uses purity.Such high purity product can use commercially available reagent, such as the reagent (purity 99.9 quality %) that can use (strain) high-purity chemical institute to make etc.
The addition means of fluorine cpd is not particularly limited, and both can add when making the magnesium oxide presoma, also can add when burning till the magnesium oxide presoma.
In order to improve luminous intensity, for magnesium oxide, the metallic element (still, except magnesium) of 1 valency, divalent, 3 valencys or 4 valencys of the amount of all right further interpolation 50～300ppm except fluorine.As such metallic element, exemplify particularly Li, Be, Na, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sb, Sn, Cs, Ba, Hf, Ta, Ir, Au, Tl, Pb, Bi, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu etc.The addition means of metallic element is not particularly limited, and both can add when making the magnesium oxide presoma, also can add when burning till the magnesium oxide presoma.For example, when the aluminium that adds as metallic element, also can be when making the magnesium oxide presoma, appropriate aluminum chloride six salt hydrates (reagent: high-purity chemical institute make) are dissolved in aqueous sodium hydroxide solution, so that aluminium is contained in the magnesium oxide of end product with the amount of 50～300ppm.The content of metallic element is that 50ppm is when above, realize that fully adding by this metallic element the luminous intensity that causes improves effect, when 300ppm is following, because the purity of magnesium oxide twinkler is higher, therefore crystallinity is good, and can guarantee enough luminous intensities, therefore be preferably the amount of 50～300ppm.
Then, (2) are burnt till the above-mentioned magnesium oxide presoma that is added with fluorine cpd and are made fluorine-containing magnesium oxide (once-firing).Process for calcining can adopt any one of closed system or open system.For example, the magnesium oxide presoma is put into crucible, and burn till after closing the lid.Temperature when burning till is preferably 600～1500 ℃ so long as the magnesium oxide presoma becomes magnesianly get final product more than 350 ℃ fully.Firing time is according to firing temperature and difference, but by considering with above-mentioned same reason, is preferably 0.5～5 hour.Heat-up rate is not particularly limited, and is about 1～10 ℃/minute.By this once-firing, form pulverous fluorine-containing magnesium oxide, but fluorine content does not descend fully still.
After the burning till of magnesium oxide presoma, the fluorine-containing magnesium oxide that (3) will obtain temporarily is cooled to normal temperature.Method of cooling can be both along temperature distribution history, cooling rate to be set as stage cooling of 1～10 ℃/minute, can be also that spontaneous combustion is cooling.
At last, (4) fluorine-containing magnesium oxide that spontaneous combustion is cooling burns till again, makes magnesium oxide twinkler of the present invention (twice firing) with this.Burn till for the second time by this, can obtain fluorine content and fully reduce, and have the fluorine-containing magnesium oxide powder of enough luminous intensities.Do not carry out and burn till for twice, and by the long-time once-firing of carrying out, when being included in fluorine content in twinkler and being reduced to amount less than 100ppm, luminous intensity descends, and carries out in addition particle growth.Therefore, can not obtain can be used as the fluorine-containing magnesium oxide powder that the UV-light releasing layer is fit to the small particle size of use.In manufacture method of the present invention, middle insert cooling and carry out twice and burn till, can access with this magnesium oxide that has enough luminous intensities and avoid particle growth when fluorine content is reduced to amount less than 100ppm.
Firing furnace in twice firing can be any one of closed system or open system.But in order effectively to reduce fluorine content, preferably in stove, atmosphere is the open system of circulation.Concrete is that the fluorine-containing magnesium oxide that will obtain in (3) is put into crucible and burnt till.Temperature when burning till is preferably 800～1700 ℃, more preferably 1000～1600 ℃ in order fully to reduce fluorine content.Firing time is according to firing temperature and difference, but in order fully to reduce fluorine content, is preferably 0.5～5 hour.Heat-up rate is not particularly limited, and is about 1～10 ℃/minute.In addition, also can and reduce fluorine content and regulate atmosphere gas when burning till or the circulation of atmosphere as purpose take the luminous intensity that improves UV-light, and be adjusted in the ratio of the air capacity of circulation in stove.
By above operation, can obtain fluorine-containing magnesium oxide twinkler of the present invention.
Therefore twinkler of the present invention can be applied to comprise in the various optical devices of plasma panel in the wavelength 200～300nm of ultra-violet region strong luminescence.
Especially twinkler of the present invention can be fit to utilize as consist of the twinkler that is arranged at the UV-light releasing layer on the dielectric material protective membrane in PDP.In order to form this UV-light releasing layer; can make as the fluorine-containing magnesium oxide powder of twinkler of the present invention and be attached directly on described protective membrane surface by sputtering method and electrostatic applications method etc.; also can make the slurry that contains this powder, thereby be coated in this slurry on said protection film and make its drying.
Embodiment:
Further described the present invention although lift following examples, the present invention is not limited to these embodiment.
In following embodiment and comparative example, according to the step measurements of the following stated various physical propertys etc.
(1) the fluorine content in magnesium oxide
Measured with the fluorine amount in the solution of dissolving with hydrochloric acid test portion and modulation by ion electrode method (device name: ionometer D-53S, HORIBA manufacturing).
(2) the accumulation 50% particle diameter (D of volume reference 50)
Measured the accumulation 50% particle diameter (D of volume reference by laser diffraction and scattering formula particle size distribution device (device name: MT3300, Nikkiso Company Limited makes) 50).
(3) measuring method of photoluminescence
Having used the Xe Excimer lamp of the exciting light that possesses emission 146nm in vacuum chamber and having measured wavelength region is the photoluminescence determination device of the spectrophotometric detector of 200～1000nm.After being arranged at the test portion box that is filled with test portion on prescribed position in vacuum chamber, the pressure in vacuum chamber is decompressed to and reaches 1.0 * 10 -1Below Pa.Then, make the test portion box move to the measuring position, and with excitation light irradiation 1000ms, measure with this luminous luminescent spectrum that radiates out from test portion.
Read the intensity of the summit that is positioned at 200～300nm ultra-violet region from the luminescent spectrum of measuring.With the intensity of summit divided by the shown intensity of reflection peak that is positioned near the laser lamp wavelength 980nm, to obtain strength ratio.
(4) magnesium oxide precursor and magnesian method for detecting purity
Magnesium oxide precursor and magnesian purity are as removing the fluorine of interpolation, and deduct from 100 quality % the impurity of measuring by the following method total amount value and calculate.
(5) measuring method of impurity element
About the impurity element (Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, In, K, Li, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Tl, V, Zn, Ti and Zr) that becomes detected object, after test portion is dissolved in acid, use ICP apparatus for analyzing luminosity (device name: SPS-5100, Seiko Instr Inc makes) to measure quality.The Cl amount is after test portion is dissolved in acid, uses spectrophotometer (device name: UV-2550, Shimadzu Seisakusho Ltd. makes) to measure quality.
The manufacturing step of the product that burn till in each embodiment and comparative example below is described.
(embodiment 1)
Be to add the magnesium fluoride that purity is 99.9 quality % (reagent: high-purity chemical institute make) in the magnesium hydroxide of 99.95 quality % so that fluorine reaches 0.105mol% with respect to magnesium in purity, and put it in crucible and close the lid.
Then, in electric furnace, the heat-up rate with 3 ℃/minute under atmospheric atmosphere heats up, and carries out the once-firing of 5 hours with the firing temperature of 1100 ℃.
Then, be cooled to normal temperature by naturally cooling.
In addition, in electric furnace, the heat-up rate with 3 ℃/minute under atmospheric atmosphere heats up, and carries out the twice firing of 1 hour with the firing temperature of 1400 ℃.
(embodiment 2)
Except carry out twice firing in gas stove, making the firing temperature of twice firing be 1200 ℃, making firing time is beyond 3 hours, carries out in the same manner with embodiment 1.
(embodiment 3)
Except the firing temperature that makes once-firing is 1200 ℃, to make firing time be 1 hour, again, twice firing is carried out in gas stove, the firing temperature that makes twice firing is beyond 1200 ℃, carries out in the same manner with embodiment 1.
(embodiment 4)
Except the firing temperature that makes once-firing is 1200 ℃, to make firing time be 1 hour, again, make beyond twice firing implements in gas stove, carry out in the same manner with embodiment 1.
(embodiment 5)
Except once-firing is carried out in gas stove, making the firing temperature of once-firing be 1200 ℃, making firing time is 1 hour, again, makes beyond twice firing implements in gas stove, carries out in the same manner with embodiment 1.
(embodiment 6)
Except the addition that makes fluorine is 1.052mol% with respect to magnesium, again, the firing temperature that makes twice firing is beyond 1200 ℃, carries out in the same manner with embodiment 5.
(embodiment 7)
Except the addition that makes fluorine is 1.052mol% with respect to magnesium, carry out in the same manner with embodiment 5.
(embodiment 8)
Except the fluorine source that makes interpolation is the Sodium Fluoride (reagent: high-purity chemical institute make) of 99 quality % purity, carry out in the same manner with embodiment 5.
(embodiment 9)
Except the fluorine source that makes interpolation is the Potassium monofluoride (reagent: high-purity chemical institute make) of 99 quality % purity, carry out in the same manner with embodiment 5.
(embodiment 10)
Be the alkaline magnesium carbonate (reagent: high-purity chemical institute make) of 99.9 quality % purity except making the magnesium oxide precursor, carry out in the same manner with embodiment 5.
(embodiment 11)
Be the magnesium acetate (reagent: high-purity chemical institute make) of 99.9 quality % purity except making the magnesium oxide precursor, carry out in the same manner with embodiment 5.
(embodiment 12)
Use has been made magnesium hydroxide with the solution that aluminum chloride six salt hydrates of 99.9 quality % purity (reagent: high-purity chemical institute make) are dissolved in sodium hydroxide (NaOH) aqueous solution, with in the fluorine-containing magnesium oxide powder of end product, contain the aluminium of 100ppm left and right with respect to magnesium.Except using this magnesium hydroxide, carry out in the same manner with embodiment 5.
(embodiment 13)
Use is dissolved in magnesium chloride (MgCl with calcium chloride two salt hydrates of 99.9 quality % purity (reagent: high-purity chemical institute make) 2) solution in the aqueous solution made magnesium hydroxide, with in the fluorine-containing magnesium oxide powder of end product, contains the calcium of 60ppm left and right with respect to magnesium.Except using this magnesium hydroxide, carry out in the same manner with embodiment 5.
(comparative example 1)
Be to add the magnesium fluoride that purity is 99.9 quality % (reagent: high-purity chemical institute make) in the magnesium hydroxide of 99.95 quality % in purity, so that fluorine reaches 0.031mol% with respect to magnesium, and put it in crucible and close the lid.
In electric furnace, under atmospheric atmosphere, heat up with the heat-up rates of 3 ℃/minute, and burnt till 1 hour with the firing temperature of 1200 ℃.
(comparative example 2)
Except the addition that makes fluorine is 0.063mol% with respect to magnesium, again, making firing time is beyond 5 hours, carries out in the same manner with comparative example 1.
(comparative example 3)
Except making firing temperature is 1500 ℃, carry out in the same manner with comparative example 1.
(comparative example 4)
Except the addition that makes fluorine is 0.105mol% with respect to magnesium, again, make burn till implement in gas stove beyond, carry out in the same manner with comparative example 1.
(comparative example 5)
Be 3 hours except making firing time, carry out in the same manner with comparative example 4.
(comparative example 6)
Except making firing temperature is 1400 ℃, carry out in the same manner with comparative example 4.
(comparative example 7)
Except the addition that makes fluorine is 1.052mol% with respect to magnesium, again, making firing temperature is beyond 1500 ℃, carries out in the same manner with comparative example 4.
(comparative example 8)
Except replacing the magnesium hydroxide as the magnesium oxide precursor, be beyond the magnesium oxide of 99.95 quality % and use purity, carry out in the same manner with comparative example 1.
(comparative example 9)
Except replacing the magnesium hydroxide as the magnesium oxide precursor, be the magnesium oxide of 99.95 quality % and use purity, and the addition that makes fluorine is beyond 0.316mol% with respect to magnesium, carry out in the same manner with comparative example 1.
Fluorine-containing magnesian each analytical results that obtains more than shown in following table 1.
[table 1]
Figure 72125DEST_PATH_IMAGE001
By table 1 as can be known, the fluorine-containing magnesium oxide that is fired into (embodiment 1～13) by two stages is that fluorine content is the lower value less than 100ppm, and the glow peak strength ratio is more than 20 simultaneously, and emitting ultraviolet light extremely consumingly.On the other hand, the fluorine-containing magnesium oxide that is fired into (comparative example 1～9) by a stage is in the situation that fluorine content is the lower value less than 100ppm, the glow peak strength ratio is less than 20, and the radiation of UV-light is inadequate, again, on the contrary in the situation that the glow peak strength ratio is more than 20, because fluorine content is more than 100ppm, therefore think the rising of the discharge ionization voltage that can not suppress PDP.

Claims (9)

1. fluorine-containing magnesium oxide twinkler is based on by electron beam or the UV-induced magnesium oxide twinkler that has glow peak in 200～300nm ultra-violet region that excites,
With respect to magnesian fluorine content less than 100ppm, and
The strength ratio that described glow peak is near the reflection peak of the laser lamp 980nm with respect to wavelength is more than 20.
2. twinkler according to claim 1, is characterized in that, be contain 50ppm with respect to magnesium oxide more than, the metallic element (still, beyond demagging) of 1 valency less than 300ppm, divalent, 3 valencys or 4 valencys and forming.
3. twinkler according to claim 2, it is characterized in that, described metallic element is one or more that select from the group who is comprised of Li, Be, Na, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sb, Sn, Cs, Ba, Hf, Ta, Ir, Au, Tl, Pb, Bi, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
4. twinkler according to claim 1, is characterized in that, is more than 99.9 quality % with the magnesian purity of calculating except fluorine.
5. according to claim 2 or 3 described twinklers, is characterized in that, is more than 99.9 quality % with the magnesian purity of calculating except fluorine and described metallic element.
6. twinkler according to claim 1 and 2, is characterized in that, described twinkler is by the accumulation 50% particle diameter (D of the volume reference of passing through laser diffraction and scattering formula particle size distribution 50) be that the fluorine-containing magnesium oxide powder that 0.8 μ m is above, 4.0 μ m are following forms.
7. twinkler according to claim 1 and 2, is characterized in that, described twinkler is used for being configured in the discharge space of plasma panel.
8. a method of making claim 1 or 2 described twinkler, is characterized in that, comprises:
In the magnesium oxide precursor, add fluorine cpd and burn till as the amount of 0.06～1.25mol% with respect to magnesium take fluorine, obtain fluorine-containing magnesian operation with this; With
After temporary transient cooling described fluorine-containing magnesium oxide, by again being fired into the operation of described twinkler.
9. method according to claim 8, is characterized in that, described magnesium oxide precursor is selected from the group who is comprised of magnesium hydroxide, alkaline magnesium carbonate, magnesiumcarbonate, magnesium acetate, magnesium nitrate and magnesium oxalate.
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