CN1101441C - Luminescent Pigments for Glazes - Google Patents
Luminescent Pigments for Glazes Download PDFInfo
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- CN1101441C CN1101441C CN 99105056 CN99105056A CN1101441C CN 1101441 C CN1101441 C CN 1101441C CN 99105056 CN99105056 CN 99105056 CN 99105056 A CN99105056 A CN 99105056A CN 1101441 C CN1101441 C CN 1101441C
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- 239000000049 pigment Substances 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 37
- 230000004907 flux Effects 0.000 claims abstract description 33
- 239000000126 substance Substances 0.000 claims abstract description 27
- 210000003298 dental enamel Anatomy 0.000 claims abstract description 23
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- LCTKKVMFUINART-UHFFFAOYSA-N [Pb].[Si].[B].[Zn] Chemical compound [Pb].[Si].[B].[Zn] LCTKKVMFUINART-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 26
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 12
- 235000019353 potassium silicate Nutrition 0.000 claims description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052689 Holmium Inorganic materials 0.000 claims description 9
- 229910052779 Neodymium Inorganic materials 0.000 claims description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 229910052684 Cerium Inorganic materials 0.000 claims description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims description 7
- 229910052691 Erbium Inorganic materials 0.000 claims description 6
- 229910017639 MgSi Inorganic materials 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 229910052775 Thulium Inorganic materials 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- 239000003086 colorant Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 239000012752 auxiliary agent Substances 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 9
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 7
- 230000005923 long-lasting effect Effects 0.000 description 7
- 239000011575 calcium Substances 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 229910052693 Europium Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 150000004645 aluminates Chemical class 0.000 description 3
- 239000001342 boswellia carteri birdw. oil Substances 0.000 description 3
- 229960000411 camphor oil Drugs 0.000 description 3
- 239000010624 camphor oil Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- ORFSSYGWXNGVFB-UHFFFAOYSA-N sodium 4-amino-6-[[4-[4-[(8-amino-1-hydroxy-5,7-disulfonaphthalen-2-yl)diazenyl]-3-methoxyphenyl]-2-methoxyphenyl]diazenyl]-5-hydroxynaphthalene-1,3-disulfonic acid Chemical compound COC1=C(C=CC(=C1)C2=CC(=C(C=C2)N=NC3=C(C4=C(C=C3)C(=CC(=C4N)S(=O)(=O)O)S(=O)(=O)O)O)OC)N=NC5=C(C6=C(C=C5)C(=CC(=C6N)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] ORFSSYGWXNGVFB-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 description 1
- LJLWNMFUZWUGPO-UHFFFAOYSA-N calcium strontium disulfide Chemical compound [S--].[S--].[Ca++].[Sr++] LJLWNMFUZWUGPO-UHFFFAOYSA-N 0.000 description 1
- KBARBLKAZCSEMJ-UHFFFAOYSA-N calcium strontium silicate Chemical compound [Ca+2].[Sr+2].[O-][Si]([O-])([O-])[O-] KBARBLKAZCSEMJ-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 229910052917 strontium silicate Inorganic materials 0.000 description 1
- QSQXISIULMTHLV-UHFFFAOYSA-N strontium;dioxido(oxo)silane Chemical compound [Sr+2].[O-][Si]([O-])=O QSQXISIULMTHLV-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Abstract
本发明制备了陶瓷、搪瓷、玻璃三种釉用发光颜料，由长余辉发光材料和基础熔剂组成。长余辉发光材料是多种离子激活的发光材料，比例3-40%；基础熔剂是硅-硼-铅-锌系统的熔剂，比例60-97%。用此颜料制造的发光陶瓷、发光搪瓷和发光玻璃制品，发光亮度高，图案清晰，颜色多样，釉面质量优良，机械性能强，化学稳定性高。The present invention prepares three kinds of luminescent pigments for glazes of ceramics, enamels and glass, which are composed of long afterglow luminescent materials and basic fluxes. The long afterglow luminescent materials are luminescent materials activated by multiple ions, with a proportion of 3-40%; the basic flux is a flux of silicon-boron-lead-zinc system, with a proportion of 60-97%. Luminescent ceramics, luminescent enamels and luminescent glass products made of the pigment have high luminescent brightness, clear patterns, various colors, excellent glaze quality, strong mechanical properties and high chemical stability.
Description
本发明属于釉用颜料技术领域。The invention belongs to the technical field of glaze pigments.
关于夜光釉，中国早在1987年，专利申请号：86101965A，1990年《景德镇陶瓷》第二期第16页和第四期第17页，专利申请号：CN94107419.6及CN98108109.6公开了一种夜光釉的制备与工艺，其所用的发光材料为ZnS型，该夜光釉的缺陷是：发光余辉时间短，亮度低，化学稳定性差。专利申请号CN98110267.0及CN98110318.9公开了关于单离子铕激活的铝酸盐型夜光釉的制备与工艺。其相对于ZnS型夜光釉的优点在于发光余辉时间长，但其釉面质量差，发光亮度低，颜色单一，且耐水化性差，使用范围窄。About luminous glaze, China as early as 1987, patent application number: 86101965A, in 1990 "Jingdezhen Ceramics" the second issue of the 16th page and the fourth issue of the 17th page, the patent application number: CN94107419.6 and CN98108109.6 disclosed a The preparation and process of a luminous glaze, the luminescent material used in it is ZnS type, the defects of the luminous glaze are: short luminous afterglow time, low brightness and poor chemical stability. Patent application numbers CN98110267.0 and CN98110318.9 disclose the preparation and process of aluminate luminous glaze activated by single ion europium. Compared with the ZnS type luminous glaze, its advantage is that the luminous afterglow time is long, but its glaze quality is poor, the luminous brightness is low, the color is single, and the hydration resistance is poor, and the application range is narrow.
本发明的目的，在于克服上述夜光釉的缺陷，制成一种使用范围广，发光性能好，化学稳定性强的釉用发光颜料。The object of the present invention is to overcome the defects of the above-mentioned luminous glaze and make a luminescent pigment for glaze with wide application range, good luminous performance and strong chemical stability.
本发明的釉用发光颜料由二部分组成：长余辉发光材料和基础熔剂。各部分重量组成为：长余辉发光材料3-40％，基础熔剂60-97％，使用时可外加0.5-5％辅助剂。The luminescent pigment for glaze of the present invention consists of two parts: long-lasting luminescent material and basic flux. The weight composition of each part is: 3-40% of long-lasting luminescent material, 60-97% of basic flux, and 0.5-5% of auxiliary agent can be added during use.
其中，长余辉发光材料是多种离子激活的碱土硅酸盐、铝酸盐和硫化钙锶。Among them, the long-lasting luminescent materials are various ion-activated alkaline earth silicates, aluminates and calcium strontium sulfide.
基础熔剂配方的化学组成如下(Wt％)：The chemical composition of basic flux formula is as follows (Wt%):
SiO2： 10-45， ZnO：2-10， SiO2 : 10-45, ZnO: 2-10,
Al2O3：0-10， SrO：1-10， Al2O3 : 0-10 , SrO: 1-10,
B2O3：2-15， TiO2：0-10，B 2 O 3 : 2-15, TiO 2 : 0-10,
K2O： 0.5-4， MgO： 0-4， K2O : 0.5-4, MgO: 0-4,
Na2O：0.5-4， BaO： 0-5， Na2O : 0.5-4, BaO: 0-5,
CaO： 0-2， PbO： 20-60。辅助剂为：Y2O3，水玻璃，羧甲基纤维，粘土中的一种或几种组合使用。CaO: 0-2, PbO: 20-60. The auxiliary agent is: Y2O3, water glass, carboxymethyl fiber, clay or a combination of several.
根据优选的原则，具体确定陶瓷、玻璃、搪瓷釉用发光颜料中优选的多离子激活的长余辉发光材料的主要化学组成表示式是：According to the preferred principle, the main chemical composition expression of the preferred multi-ion activated long-lasting luminescent material in the luminescent pigment for ceramics, glass and enamel glaze is:
1.(Sr1-zCaz)2MgSi2O7：EuxLny 1. (Sr 1-z Ca z ) 2 MgSi 2 O 7 : Eu x Ln y
其中，Ln代表La、Ce、Dy、Tm、Ho、Nd、Er、Sb、Bi中的一种或多种元素组合；Among them, Ln represents one or more element combinations in La, Ce, Dy, Tm, Ho, Nd, Er, Sb, Bi;
z代表系数0≤z≤1，z represents the coefficient 0≤z≤1,
x，y代表摩尔系数0.0001≤x≤0.2，x, y represents the molar coefficient 0.0001≤x≤0.2,
0.0001≤y≤0.3，0.0001≤y≤0.3,
随Z从0到1变化，材料呈兰-兰绿-绿-黄绿-黄发光变化。As Z changes from 0 to 1, the material exhibits blue-blue-green-green-yellow-green-yellow luminescence.
2.(Sr1-zCaz)3MgSi2O8：EuxLny 2. (Sr 1-z Ca z ) 3 MgSi 2 O 8 : Eu x Ln y
其中，Ln代表La、Ce、Dy、Tm、Ho、Nd、Er、Sb、Among them, Ln represents La, Ce, Dy, Tm, Ho, Nd, Er, Sb,
Bi中的一种或多种元素组合；Combinations of one or more elements in Bi;
z代表系数0≤z≤1z represents the coefficient 0≤z≤1
x，y代表摩尔系数0.0001≤x≤0.2，x, y represents the molar coefficient 0.0001≤x≤0.2,
0.0001≤y≤0.3随Z从0到1变化，材料呈兰-兰绿-绿-黄绿-黄发光变化。 0.0001≤y≤0.3 As Z changes from 0 to 1, the material exhibits a blue-blue-green-green-yellow-green-yellow luminescent change.
3.MAl2O4：EuxLny 3. MAl 2 O 4 : Eu x Ln y
其中Ln代表La、Ce、Dy、Ho、Nd、Er一种或多种元素组合；Wherein Ln represents La, Ce, Dy, Ho, Nd, Er one or more combination of elements;
M代表Sr、Ca、Mg、Ba中一种或2种以上组合；M represents one or more combinations of Sr, Ca, Mg, Ba;
x，y代表摩尔系数0.0001≤x≤0.15，x, y represents the molar coefficient 0.0001≤x≤0.15,
0.0001≤y≤0.2，0.0001≤y≤0.2,
随M不同元素和元素组合，材料呈紫-兰-黄绿色发光变化。With the different elements and element combinations of M, the material shows purple-blue-yellow-green luminous change.
4.M4Al14O25：EuxLny 4. M 4 Al 14 O 25 : Eu x Ln y
其中Ln代表Pr、Ce、Dy、Ho、Nd、Er一种或多种元素组合；Where Ln represents a combination of one or more elements of Pr, Ce, Dy, Ho, Nd, Er;
M代表SrCa中一种或2种元素组合；M represents one or a combination of two elements in SrCa;
x，y代表摩尔系数0.0001≤x≤0.25，x, y represents the molar coefficient 0.0001≤x≤0.25,
0.0001≤y≤0.3，该材料呈兰绿色发光。 0.0001≤y≤0.3, the material emits blue-green light.
5.(Ca1-zSrz)S：EuxLny 5. (Ca 1-z Srz)S: Eu x Ln y
其中Ln代表Er、Dy、La、Tm、Y一种或多种元素组合；Wherein Ln represents Er, Dy, La, Tm, Y one or more element combinations;
Z代表系数0≤z≤1，Z represents the coefficient 0≤z≤1,
x，y代表摩尔系数0.00001≤x≤0.2，x, y represents the molar coefficient 0.00001≤x≤0.2,
0.00001≤y≤0.15，随Z从0到1变化，材料呈红-橙色发光变化。根据陶瓷釉、搪瓷釉和玻璃釉的物化性能不同，优选基础熔剂组成范围和各部分化学组成范围及辅助剂如下： 0.00001≤y≤0.15, as Z changes from 0 to 1, the material exhibits a red-orange glow. According to the different physical and chemical properties of ceramic glaze, enamel glaze and glass glaze, the preferred basic flux composition range and the chemical composition range of each part and auxiliary agents are as follows:
1、陶瓷釉用发光颜料1. Luminous pigments for ceramic glazes
基础熔剂化学组成(Wt％)：Basic flux chemical composition (Wt%):
SiO2： 12-40， ZnO： 2-8， SiO2 : 12-40, ZnO: 2-8,
Al2O3：1-10， SrO： 2-10， Al2O3 : 1-10 , SrO: 2-10,
B2O3： 2-10， TiO2：0-2，B 2 O 3 : 2-10, TiO 2 : 0-2,
K2O： 0.5-2， MgO： 0-4， K2O : 0.5-2, MgO: 0-4,
Na2O： 0.5-2， BaO： 0-5， Na2O : 0.5-2, BaO: 0-5,
CaO： 1-2， PbO： 30-60；CaO: 1-2, PbO: 30-60;
辅助剂为：水玻璃，羧甲基纤维素中的一种或两种组合使用。釉用发光颜料各部分组成范围：The auxiliary agent is: one or both of water glass and carboxymethyl cellulose are used in combination. The composition range of each part of the luminescent pigment for glaze:
长余辉发光材料：10-30％；基础熔剂：70-90％；使用时外加辅助剂0.5-5％。Long afterglow luminescent material: 10-30%; basic flux: 70-90%; add auxiliary agent 0.5-5% when used.
2、搪瓷用发光颜料2. Luminous pigments for enamel
基础熔剂化学组成(Wt％)：Basic flux chemical composition (Wt%):
SiO2： 10-35， ZnO： 2-6， SiO2 : 10-35, ZnO: 2-6,
Al2O3：0-5， SrO： 1-5， Al2O3 : 0-5, SrO: 1-5,
B2O3： 4-10， TiO2：0-10，B 2 O 3 : 4-10, TiO 2 : 0-10,
K2O： 0.5-2， MgO： 0-4， K2O : 0.5-2, MgO: 0-4,
Na2O： 0.5-2， BaO： 0-5， Na2O : 0.5-2, BaO: 0-5,
CaO： 0-1， PbO： 20-50；CaO: 0-1, PbO: 20-50;
辅助剂为：Y2O3，水玻璃，羧甲基纤维，粘土中的一种或几种组合使用。用。The auxiliary agent is: Y2O3, water glass, carboxymethyl fiber, clay or a combination of several. use.
釉用发光颜料各部分组成范围：The composition range of each part of the luminescent pigment for glaze:
长余辉发光材料：5-40％；基础熔剂：60-95％；使用时外加辅助剂0.5-5％。Long afterglow luminescent material: 5-40%; basic flux: 60-95%; add auxiliary agent 0.5-5% when used.
3、玻璃釉用发光颜料3. Luminescent pigments for glass glaze
基础熔剂化学组成(wt％)Basic flux chemical composition (wt%)
SiO2： 10-36 ZnO： 2-8SiO 2 : 10-36 ZnO: 2-8
Al2O3：1-5 SrO： 2-10Al 2 O 3 : 1-5 SrO: 2-10
B2O3： 5-10 TiO2：0-2B 2 O 3 : 5-10 TiO 2 : 0-2
K2O： 0.5-2 MgO： 0-4K 2 O: 0.5-2 MgO: 0-4
Na2O： 1-2 BaO： 0-5 Na2O : 1-2 BaO: 0-5
CaO： 0-1 PbO： 20-60CaO: 0-1 PbO: 20-60
辅助剂为：水玻璃，羧甲基纤维素Auxiliaries are: water glass, carboxymethyl cellulose
发光颜料各部分组成范围：The composition range of each part of the luminous pigment:
长余辉发光材料：10-25％；基础熔剂：75-90％；使用时外加辅助剂0.5-5％。Long afterglow luminescent material: 10-25%; basic flux: 75-90%; add auxiliary agent 0.5-5% when used.
釉用发光颜料的制备工艺步骤为：The preparation process steps of the luminescent pigment for glaze are as follows:
1.基础熔剂的制备1. Preparation of base flux
按基础熔剂的组成配料、混匀，在950℃-1150℃之间溶制，保温0.5-3h，水淬、烘干、粉碎过300目。According to the composition of the basic flux, mix and mix, melt at 950°C-1150°C, keep warm for 0.5-3h, quench in water, dry, and crush through 300 mesh.
2.釉用发光颜料的合成2. Synthesis of Luminescent Pigments for Glazes
将制得的基础熔剂与长余辉发光材料按比例混合，球磨混匀即制得釉用发光颜料。The prepared basic flux and the long-lasting luminescent material are mixed in proportion, and the luminescent pigment for glaze is obtained by ball milling and mixing evenly.
3.所制得的釉用发光颜料在900℃以下使用。3. The prepared luminous pigment for glaze is used below 900°C.
所选用的长余辉发光材料是含有多种离子激活的硅酸盐、铝酸盐，易于与基础溶剂结合；恰当的基础溶剂的选择对其具有增强和保护作用。本发明与现有技术相比，其优点在于：The selected long-lasting luminescent material contains a variety of ion-activated silicates and aluminates, which are easy to combine with the base solvent; the selection of an appropriate base solvent can enhance and protect it. Compared with the prior art, the present invention has the advantages of:
1.拓宽发光材料在硅酸盐领域的使用范围，可制成具有高发光性能的陶瓷、玻璃、搪瓷制品。1. Broaden the scope of use of luminescent materials in the field of silicate, and can be made into ceramics, glass, and enamel products with high luminescent properties.
2.产品发光亮度高，图案清晰，颜色多样。2. The product has high luminous brightness, clear patterns and various colors.
3.釉面质量好，机械性能强，化学稳定性好。3. The quality of the glaze surface is good, the mechanical properties are strong, and the chemical stability is good.
为说明本发明的使用，举应用实例如下：For illustrating the use of the present invention, give application example as follows:
实施例1：陶瓷釉用发光颜料Embodiment 1: luminescent pigment for ceramic glaze
长余辉发光材料：采用Eu、Dy、Bi三种离子激活的钙锶硅酸盐兰色发光材料，主要化学组成表示式：(Ca0.9Sr0.12)MgSi2O7：Eu0.06Dy0.15Bi0.01基础熔剂的制备Long afterglow luminescent material: calcium strontium silicate blue luminescent material activated by Eu, Dy and Bi ions, the main chemical composition expression: (Ca 0.9 Sr 0.12 ) MgSi 2 O 7 : Eu 0.06 Dy 0.15 Bi 0.01 basis Flux preparation
基础熔剂化学组成：Basic Flux Chemical Composition:
SiO2： 30， ZnO：5， SiO2 : 30, ZnO: 5,
Al2O3：2， SrO：5，Al 2 O 3 : 2, SrO: 5,
B2O3： 6， Na2O：0.8， B2O3 : 6 , Na2O : 0.8,
K2O： 0.5， CaO：0.5， K2O : 0.5, CaO: 0.5,
PbO： 50.2，PbO: 50.2,
其中B2O3由硼酸或硼砂引入，Al2O3主要由长石引入，按基础熔剂的化学组成计算出相应的原料组成配方，准确称量，混均，在980℃下保温50min制得熔块后，干法球磨，过300目筛，即制得熔剂。Among them, B 2 O 3 is introduced by boric acid or borax, and Al 2 O 3 is mainly introduced by feldspar. According to the chemical composition of the basic flux, the corresponding raw material composition formula is calculated, accurately weighed, mixed, and kept at 980°C for 50 minutes. After fritting, dry ball milling and passing through a 300 mesh sieve to obtain flux.
辅助剂：水玻璃(模数在2.3-3.3之间)。Auxiliary agent: water glass (modulus between 2.3-3.3).
将发光材料，基础熔剂，按10％∶90％的比例充分混合，制得陶瓷兰色釉用发光颜料。使用时再外加1.2％的水玻璃和50％的水(或40％乳香油和樟脑油或印油)即制得可做釉上(下)彩绘或印刷的陶瓷釉用发光颜料。The luminous material and the basic flux are fully mixed according to the ratio of 10%:90% to prepare the luminescent pigment for ceramic blue glaze. When in use, add 1.2% water glass and 50% water (or 40% frankincense oil and camphor oil or printing oil) to obtain a luminescent pigment for ceramic glaze that can be used for overglaze (under) painting or printing.
实施例2：搪瓷釉用发光颜料Embodiment 2: luminescent pigment for enamel glaze
长余辉发光材料：采用Eu、Dy、La激活的锶钙铝酸盐兰绿发光材料，主要化学组成表示式为：(Sr0.85Ca0.15)4Al14O25：Eu0.06Dy0.09La0.02 Long afterglow luminescent material: Strontium calcium aluminate blue-green luminescent material activated by Eu, Dy, La, the main chemical composition expression is: (Sr 0.85 Ca 0.15 ) 4 Al 14 O 25 : Eu 0.06 Dy 0.09 La 0.02
基础熔制的制备Preparation of basic melting
基础熔制化学组成(Wt％)：Basic melting chemical composition (Wt%):
SiO2： 32， ZnO：2， SiO2 : 32, ZnO: 2,
Al2O3：1， SrO：2，Al 2 O 3 : 1, SrO: 2,
B2O3： 10， K2O：0.5， B2O3 : 10 , K2O : 0.5,
Na2O： 1.5， CaO：0.5， Na2O : 1.5, CaO: 0.5,
PbO： 51。除熔制熔块时在900℃保温1h外，其制备方法同实施例1辅助剂：水玻璃(模数在2.3-3.3之间)PbO: 51. Except that the frit is kept at 900°C for 1h, its preparation method is the same as in Example 1. Auxiliary agent: water glass (modulus between 2.3-3.3)
将发光材料，基础熔剂按12％∶88％比例充分混合，制得搪瓷釉用兰绿色发光颜料。使用时再外加入1.5％的水玻璃和40％的水(或40％的乳香油和樟脑油或印油)即可调制成搪瓷釉用发光颜料。The luminescent material and the basic flux are fully mixed at a ratio of 12%:88% to prepare a blue-green luminescent pigment for enamel glaze. When in use, add 1.5% water glass and 40% water (or 40% frankincense oil and camphor oil or printing oil) to prepare the luminous pigment for enamel glaze.
实施例3玻璃釉用发光颜料Embodiment 3 luminescent pigments for glass glaze
长余辉发光材料：采用Eu、Ho、Nd激活的锶硅酸盐纯兰色发光材料，主要化学组成：Sr3MgSi2O8：Eu0.1Ho0.05Nd0.05基础熔剂的制备Long-lasting luminescent material: Strontium silicate pure blue luminescent material activated by Eu, Ho, Nd, main chemical composition: Sr 3 MgSi 2 O 8 : Preparation of basic flux of Eu 0.1 Ho 0.05 Nd 0.05
基础熔剂的化学组成(Wt％)：Chemical composition of base flux (Wt%):
SiO2： 20， ZnO： 8， SiO2 : 20, ZnO: 8,
Al2O3：0.5， SrO： 1， Al2O3 : 0.5 , SrO: 1,
B2O3： 10， TiO2：10，B 2 O 3 : 10, TiO 2 : 10,
K2O： 0.5， MgO： 1， K2O : 0.5, MgO: 1,
Na2O： 0.5， PbO： 49.5。除熔制熔块时在1050℃保温1h外，其制备方法同实施例1。 Na2O : 0.5, PbO: 49.5. Its preparation method is the same as that of Example 1, except that it is kept at 1050° C. for 1 h when melting the frit.
辅助剂：水玻璃(模数在2.3-3.3之间)。Auxiliary agent: water glass (modulus between 2.3-3.3).
将发光材料和基础熔剂按15％∶85％比例充分混合，制得玻璃釉用纯兰色发光颜料。使用时再加入1.5％的水玻璃和40％的水(或40％的乳香油和樟脑油或印油)即可调制成玻璃釉用发光颜料。The luminescent material and the basic flux are fully mixed at a ratio of 15%:85% to prepare a pure blue luminescent pigment for glass glaze. When in use, add 1.5% water glass and 40% water (or 40% frankincense oil and camphor oil or printing oil) to prepare the luminescent pigment for glass glaze.
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| EP3515997A1 (en) * | 2016-09-20 | 2019-07-31 | Stoelzle Masnieres Parfumerie | Item at least partially coated with at least one layer of luminescent coating |
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| CN100586885C (en) * | 2003-10-04 | 2010-02-03 | 大连路明发光科技股份有限公司 | Method for manufacturing long-afterglow luminescent glass |
| CN101723588B (en) * | 2008-10-14 | 2012-12-19 | 浙江开尔实业有限公司 | Long-persistence luminous enameled plate and preparation method thereof |
| CN102030472B (en) * | 2009-09-28 | 2012-09-05 | 海洋王照明科技股份有限公司 | Borate luminescent glass and preparation method thereof |
| CN102936499B (en) * | 2012-10-19 | 2014-07-02 | 深圳市永丰源瓷业有限公司 | High temperature resistance anti-counterfeiting composition and preparation method thereof |
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| EP3515997A1 (en) * | 2016-09-20 | 2019-07-31 | Stoelzle Masnieres Parfumerie | Item at least partially coated with at least one layer of luminescent coating |
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