CN108117260B - The preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing - Google Patents

The preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing Download PDF

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CN108117260B
CN108117260B CN201711437992.4A CN201711437992A CN108117260B CN 108117260 B CN108117260 B CN 108117260B CN 201711437992 A CN201711437992 A CN 201711437992A CN 108117260 B CN108117260 B CN 108117260B
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glaze
mass parts
accumulating type
ceramic material
glass ceramic
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CN108117260A (en
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宋维伟
李蕊
王延泽
王中恺
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Jiangxi Geely Ceramics Co ltd
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Zhuji City Fire Industry Design Studio
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions

Abstract

The invention discloses a kind of preparation methods of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing, and the accumulating type luminous glaze glass ceramic material is by SrAl2O4:Eu2+,Dy3+It is prepared with parent glaze；Wherein, the parent glaze by 35-50 mass parts B2O3, 2-5 mass parts ZrO2, 5-20 mass parts TeO2, 15-20 mass parts ZnO, 20-30 mass parts Na2O2, 5-10 mass parts Al2O3With the La of 2-5 mass parts2O3It is prepared, the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing of the invention is sintered by low temperature (450-500 degrees Celsius), accumulating type luminous glaze glass ceramic coating made of accumulating type luminous glaze glass ceramic material by the low temperature of glaze firing, accumulating type luminous glaze glass ceramic coating can also continue to shine after 750 DEG C of high temperature sinterings.

Description

The preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing
(the present patent application is parent application " the accumulating type luminous glaze glass ceramic material and preparation method of low temperature of glaze firing And its application " divisional application, parent application application No. is 2015110317385, the applying date is on December 30th, 2016.)
Technical field
The invention belongs to new material technology fields, relate in particular to a kind of accumulating type luminous glaze glass of low temperature of glaze firing Ceramic material and preparation method and applications.
Background technique
The mark of Noctilucent safety fire-fighting made of Noctilucent material indicates evacuation side with obvious text, distinct arrow mark Evacuation safety when occurring to, effective guarantee fire.Currently used Noctilucent safety mark is with luminescent coating and plastics system , moment will deform after these security against fires for containing organic components mark is burnt by open fire in a fire, it turns to dust and ashes, It loses luminous.It loses the effect for guiding correct escape route soon in a fire, protection people's life safety cannot be played Effect.In order to solve this technical problem, patent (104003757 A of CN) discloses a kind of production of Luminous fire mark Method, in ceramic plane with transparent polishing dry granular and luminescent powder silk-screen at luminous glaze glass ceramic material pattern, but it is used It is transparent polishing dry granular basis glaze firing temperature it is higher (1200 degrees Celsius), at such high temperatures, Noctilucent material easily with Parent glaze reacts, and influences the luminous intensity of noctilucence powder material, to influence the illumination effect of Noctilucent safety mark.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of accumulating type luminous glaze glass of low temperature of glaze firing Ceramic material and preparation method and applications.
The purpose of the present invention is what is be achieved by following technical proposals.
A kind of accumulating type luminous glaze glass ceramic material of low temperature of glaze firing, by SrAl2O4:Eu2+,Dy3+With parent glaze system It is standby to form, by mass, SrAl2O4:Eu2+,Dy3+And the ratio of parent glaze is 1:3；Wherein, the parent glaze is by 35-50 mass parts B2O3, 2-5 mass parts ZrO2, 5-20 mass parts TeO2, 15-20 mass parts ZnO, 20-30 mass parts Na2O2、5- The Al of 10 mass parts2O3With the La of 2-5 mass parts2O3It is prepared.
In the above-mentioned technical solutions, the B2O3For 40-45 mass parts, ZrO2For 3-4 mass parts, TeO2For 10-15 mass Part, ZnO are 16-19 mass parts, Na2O2For 22-27 mass parts, Al2O3For 6-9 mass parts and La2O3For 3-6 mass parts.
A kind of preparation method of the accumulating type luminous glaze glass ceramic material of above-mentioned low temperature of glaze firing, gives as steps described below With preparation:
1) by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled in proportion uniformly mixed, is put into high temperature furnace In in 2-4 hour of 900-1200 DEG C of sintering, obtain forerunner's glass；Forerunner's glass machinery is crushed to glass particle, is put into ball It carries out ball milling 1-12 hours in grinding machine, is sieved after ball milling with the sieve of 300-400 mesh, parent glaze powder is made；
2) by 1) gained parent glaze powder and SrAl2O4:Eu2+,Dy3+It mixes to uniform, is sintered under 450-500 degrees Celsius 15-45 minutes to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing.
In the above-mentioned technical solutions, by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled to mixing in proportion Uniformly, it is put into high temperature furnace in 2-4 hour of 1000-1150 DEG C of sintering, obtains forerunner's glass.
In the above-mentioned technical solutions, by 1) gained parent glaze powder and SrAl2O4:Eu2+,Dy3+It mixes to uniform, in 450- 20-30 minutes are sintered under 500 degrees Celsius to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing.
A kind of application of the accumulating type luminous glaze glass ceramic material of above-mentioned low temperature of glaze firing, by the low temperature of glaze firing Accumulating type luminous glaze glass ceramic material is mixed with glycerol, is passed through silk-screen printing after mixing, is brushed or be sprayed on ceramic tile surface On, accumulating type luminous glaze glass ceramic coating is made, passes through screen printing in the upper surface of described accumulating type luminous glaze glass-ceramic layer One layer of covering basic glaze layer is brushed or sprayed to brush；The ceramic tile is put into high temperature furnace at 450-550 DEG C of sintering 5-10 points Clock.
In the above-mentioned technical solutions, by mass, the ratio of the accumulating type luminous glaze glass ceramic material and glycerol is 9: 1。
The accumulating type luminous glaze glass ceramic material of low temperature of glaze firing of the invention is by (450-500 degrees Celsius) of low temperature burning It ties, accumulating type luminous glaze glass ceramics made of the accumulating type luminous glaze glass ceramic material by the low temperature of glaze firing applies Layer, accumulating type luminous glaze glass ceramic coating can also continue to shine after 750 DEG C of high temperature sinterings.
Detailed description of the invention
Fig. 1 is that the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing of the invention is brushed to the transmitting after potsherd Spectrogram；
Fig. 2 is that the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing of the invention is brushed to the transmitting after potsherd Spectrogram；
Fig. 3 is that the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing of the invention is brushed to the transmitting after potsherd Spectrogram；
Fig. 4 is that the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing of the invention is brushed to the transmitting after potsherd Spectrogram.
Specific embodiment
In the present embodiment, raw material B2O3、ZrO2、TeO2、ZnO、Al2O3、Na2O2And La2O3It is purchased from Aladdin examination Agent, wherein B2O3Article No. is B108406-500g, TeO2Article No. is T103864, and ZnO article No. is Z111836, Al2O3Article No. is A140802, La2O3Article No. is L103872, Na2O2Article No. is S100113.Test equipment: F-4600 sepectrophotofluorometer (day Vertical high and new technology company), 320 nanometers of ultraviolet excitation sample of test in the present embodiment.
SrAl2O4:Eu2+,Dy3+Preparation method: will strontium carbonate (99.2%), be added in aluminum oxide (99.99%) Analytically pure Eu2O3, Dy2O3After be uniformly mixed, at 1300 DEG C in reducing atmosphere 2 hours be burnt into, crushed, shone Material sample.Wherein, by the meter of substance, strontium carbonate (99.2%), aluminum oxide (99.99%), Eu2O3And Dy2O3Ratio For 9:10:0.1:0.4.
Application method: the accumulating type luminous glaze glass ceramic material of the low temperature of glaze firing is mixed with glycerol, after mixing One layer is brushed on ceramic tile surface, accumulating type luminous glaze glass ceramic coating is made, in the accumulating type luminous glaze glass ceramics The upper surface of layer is by brushing one layer of covering basic glaze layer；The ceramic tile is put into high temperature furnace at 450-550 DEG C of sintering 5-10 points Clock, wherein by mass, the ratio of the accumulating type luminous glaze glass ceramic material and glycerol is 9:1.
In an embodiment of the present invention, 1 mass parts are 1g.
With reference to the accompanying drawings and examples to the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing of the invention into Row is described in detail.
Embodiment 1
1) by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled in proportion uniformly mixed, is put into high temperature furnace In in 1000 DEG C of 3 hours of sintering, obtain forerunner's glass；Forerunner's glass machinery is crushed to glass particle, is put into ball mill It carries out ball milling 6 hours, is sieved after ball milling with the sieve of 300 mesh, parent glaze powder is made；Wherein, the parent glaze is by 37 The B of mass parts2O3, 2 mass parts ZrO2, 7 mass parts TeO2, the ZnO of 16 mass parts, 22 mass parts Na2O2, 6 mass parts Al2O3With the La of 2 mass parts2O3It is prepared.
2) by 1) resulting parent glaze powder and SrAl2O4:Eu2+,Dy3+It mixes to uniform, is burnt under 500 degrees Celsius Knot 25 minutes to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing, wherein by mass, SrAl2O4: Eu2+,Dy3+And the ratio of parent glaze is 1:3.
Brushing accumulating type luminous glaze glass ceramic material made from embodiment 1 to diameter according to above-mentioned application method is 3 Centimetre, with a thickness of on 1 millimeter of potsherd, potsherd is put into F-4600 sepectrophotofluorometer and is tested, emit light Spectrum such as the curve 1 in attached drawing 1.
After test, above-mentioned potsherd is put into Muffle furnace, is sintered 30 minutes at 750 degrees c, it is naturally cold after taking-up But to 20-25 DEG C of room temperature, which is put into F-4600 sepectrophotofluorometer and is tested, emission spectrum such as attached drawing 1 In curve 2.
As seen from the figure, compared to curve 1, the luminous intensity of curve 2 has dropped 26%, illustrates accumulating type noctilucence of the invention Glaze glass ceramic material can still shine after oversintering,
Embodiment 2
1) by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled in proportion uniformly mixed, is put into high temperature furnace In in 1000 DEG C of 3 hours of sintering, obtain forerunner's glass；Forerunner's glass machinery is crushed to glass particle, is put into ball mill It carries out ball milling 6 hours, is sieved after ball milling with the sieve of 300 mesh, parent glaze powder is made；Wherein, the parent glaze is by 42 The B of mass parts2O3, 3 mass parts ZrO2, 12 mass parts TeO2, the ZnO of 17 mass parts, 24 mass parts Na2O2, 7 mass parts Al2O3With the La of 3 mass parts2O3It is prepared.
2) by 1) resulting parent glaze powder and SrAl2O4:Eu2+,Dy3+It mixes to uniform, is burnt under 500 degrees Celsius Knot 25 minutes to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing, wherein by mass, SrAl2O4: Eu2+,Dy3+And the ratio of parent glaze is 1:3.Curve 2 in its emission spectrum such as attached drawing 1.
Brushing accumulating type luminous glaze glass ceramic material made from embodiment 2 to diameter according to above-mentioned application method is 3 Centimetre, with a thickness of on 1 millimeter of potsherd, potsherd is put into F-4600 sepectrophotofluorometer and is tested, emit light Spectrum such as the curve 1 in attached drawing 2.
After test, above-mentioned potsherd is put into Muffle furnace, calcination 30 minutes, naturally cold after taking-up at 750 degrees c But to 20-25 DEG C of room temperature, which is put into F-4600 sepectrophotofluorometer and is tested, emission spectrum such as attached drawing 2 In curve 2.
As seen from the figure, compared to curve 1, the luminous intensity of curve 2 has dropped 17%, illustrates accumulating type noctilucence of the invention Glaze glass ceramic material can still shine after oversintering,
Embodiment 3
1) by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled in proportion uniformly mixed, is put into high temperature furnace In in 1000 DEG C of 3 hours of sintering, obtain forerunner's glass；Forerunner's glass machinery is crushed to glass particle, is put into ball mill It carries out ball milling 6 hours, is sieved after ball milling with the sieve of 300 mesh, parent glaze powder is made；Wherein, the parent glaze is by 46 The B of mass parts2O3, 4 mass parts ZrO2, 17 mass parts TeO2, the ZnO of 18 mass parts, 26 mass parts Na2O2, 8 mass parts Al2O3With the La of 4 mass parts2O3It is prepared.
2) by 1) resulting parent glaze powder and SrAl2O4:Eu2+,Dy3+It mixes to uniform, is burnt under 500 degrees Celsius Knot 25 minutes to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing, wherein by mass, SrAl2O4: Eu2+,Dy3+And the ratio of parent glaze is 1:3.Curve 3 in its emission spectrum such as attached drawing 1.
Brushing accumulating type luminous glaze glass ceramic material made from embodiment 1 to diameter according to above-mentioned application method is 3 Centimetre, with a thickness of on 1 millimeter of potsherd, potsherd is put into F-4600 sepectrophotofluorometer and is tested, emit light Spectrum such as the curve 1 in attached drawing 3.
After test, above-mentioned potsherd is put into Muffle furnace, calcination 30 minutes, naturally cold after taking-up at 750 degrees c But to 20-25 DEG C of room temperature, which is put into F-4600 sepectrophotofluorometer and is tested, emission spectrum such as attached drawing 3 In curve 2.
As seen from the figure, compared to curve 1, the luminous intensity of curve 2 has dropped 11%, illustrates accumulating type noctilucence of the invention Glaze glass ceramic material can still shine after oversintering,
Embodiment 4
1) by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled in proportion uniformly mixed, is put into high temperature furnace In in 1000 DEG C of 3 hours of sintering, obtain forerunner's glass；Forerunner's glass machinery is crushed to glass particle, is put into ball mill It carries out ball milling 6 hours, is sieved after ball milling with the sieve of 300 mesh, parent glaze powder is made；Wherein, the parent glaze is by 49 The B of mass parts2O3, 5 mass parts ZrO2, 19 mass parts TeO2, the ZnO of 19 mass parts, 28 mass parts Na2O2, 9 mass parts Al2O3With the La of 5 mass parts2O3It is prepared.
2) by 1) resulting parent glaze powder and SrAl2O4:Eu2+,Dy3+It mixes to uniform, is burnt under 500 degrees Celsius Knot 25 minutes to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing, wherein by mass, SrAl2O4: Eu2+,Dy3+And the ratio of parent glaze is 1:3.Curve 4 in its emission spectrum such as attached drawing 1.
Brushing accumulating type luminous glaze glass ceramic material made from embodiment 1 to diameter according to above-mentioned application method is 3 Centimetre, with a thickness of on 1 millimeter of potsherd, potsherd is put into F-4600 sepectrophotofluorometer and is tested, emit light Spectrum such as the curve 1 in attached drawing 4.
After test, above-mentioned potsherd is put into Muffle furnace, calcination 30 minutes, naturally cold after taking-up at 750 degrees c But to 20-25 DEG C of room temperature, which is put into F-4600 sepectrophotofluorometer and is tested, emission spectrum such as attached drawing 4 In curve 2.
As seen from the figure, compared to curve 1, the luminous intensity of curve 2 has dropped 73%, illustrates accumulating type noctilucence of the invention Glaze glass ceramic material can still shine after oversintering,
By above-mentioned test result, it is found that accumulating type luminous glaze glass ceramic material of the invention is by low temperature, (450-500 is taken the photograph Family name's degree) it is sintered, accumulating type luminous glaze glass made of the accumulating type luminous glaze glass ceramic material by the low temperature of glaze firing Ceramic coating, accumulating type luminous glaze glass ceramic coating can also continue to shine at after high temperature sintering (500 DEG C).
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal Fall into protection scope of the present invention.

Claims (4)

1. a kind of preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing, which is characterized in that low glaze firing temperature The accumulating type luminous glaze glass ceramic material of degree is by SrAl2O4:Eu2+,Dy3+It is prepared with parent glaze, by mass, SrAl2O4:Eu2+,Dy3+And the ratio of parent glaze is 1:3；Wherein, the parent glaze by 35-50 mass parts B2O3, 2-5 mass parts ZrO2, 5-20 mass parts TeO2, 15-20 mass parts ZnO, 20-30 mass parts Na2O2, 5-10 mass parts Al2O3With The La of 2-5 mass parts2O3It is prepared；
The accumulating type luminous glaze glass ceramic material of low temperature of glaze firing is prepared as steps described below:
1) by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled to uniformly mixed, is put into high temperature furnace in proportion 2-4 hour of 900-1200 DEG C of sintering, obtain forerunner's glass；Forerunner's glass machinery is crushed to glass particle, is put into ball mill Middle progress ball milling 1-12 hours, is sieved after ball milling with the sieve of 300-400 mesh, and parent glaze is made；
2) by 1) gained parent glaze and SrAl2O4:Eu2+,Dy3+It mixes to uniform, 15-45 points of sintering under 450-500 degrees Celsius Clock is to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing.
2. the preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing according to claim 1, special Sign is, the B2O3For 40-45 mass parts, ZrO2For 3-4 mass parts, TeO2It is 16-19 mass for 10-15 mass parts, ZnO Part, Na2O2For 22-27 mass parts, Al2O3For 6-9 mass parts and La2O3For 3-6 mass parts.
3. the preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing according to claim 2, special Sign is, by B2O3、ZrO2、TeO2、ZnO、Na2O2、Al2O3And La2O3It is milled to uniformly mixed, is put into high temperature furnace in proportion In 2-4 hour of 1000-1150 DEG C of sintering, forerunner's glass is obtained.
4. the preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing according to claim 3, special Sign is, by 1) gained parent glaze and SrAl2O4:Eu2+,Dy3+It mixes to uniform, is sintered 20- under 450-500 degrees Celsius 30 minutes to get the accumulating type luminous glaze glass ceramic material for arriving the low temperature of glaze firing.
CN201711437992.4A 2015-12-30 2015-12-30 The preparation method of the accumulating type luminous glaze glass ceramic material of low temperature of glaze firing Expired - Fee Related CN108117260B (en)

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