CN1192077C - Luminous jade and preparing process thereof - Google Patents

Luminous jade and preparing process thereof Download PDF

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CN1192077C
CN1192077C CNB99126777XA CN99126777A CN1192077C CN 1192077 C CN1192077 C CN 1192077C CN B99126777X A CNB99126777X A CN B99126777XA CN 99126777 A CN99126777 A CN 99126777A CN 1192077 C CN1192077 C CN 1192077C
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jade
luminous
elements
combination
raw material
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CN1270151A (en
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肖志国
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Abstract

The present invention relates to a luminous jade whose expression formula of the main chemical components is aMbeta*bM'beta*cSiO2*dAl2O3*eEu2O3*fB2O3*gLn2O3*hZrO2, wherein the M is the combination of one element or a plurality of elements of Ca, Sr , Ba, Mg, Zn and Cd; the M' is the combination of one element or a plurality of elements of Be, Mg , Zn and Cd; the beta is the combination of one element or two elements of O and S; the Ln is the combination of one element or a plurality of elements of Ce, Pr , La, Dy, Ho, Nd , Er, Bi, Ga, Sb , Lu, Y, Mn , Mo, Cr, Sn, Cu and Tm; the a , the b, the c, the d, the e, the f, the g and the h are respectively mole coefficients. Compounds containing the elements are sintered at the high temperature after being mixed, so the luminous jade is formed. The luminous jade has the advantages of compact, exquisite and tough texture, and can make luminous action for a long time after the luminous jade is irradiated by the light. In addition, the luminous jade can become bright, smooth and clean after the luminous jade is polished.

Description

Luminous jade
Technical field
What the present invention relates to is artificial luminescent jade technology, particularly about artificial luminescent jade and the manufacture method thereof of holding light-luminescent properties arranged.
Background technology
Jade is meant hardness below 3 degree above 7 are spent, quality densification, tough and tensile natural crystal, through being processed into various artworks, have very high view and admire, use and reserve value.But jade is natural goods, resource-constrained, and it costs an arm and a leg and embarrasses popular acceptance in addition.The good wine of grape described in classic poetry luminous wine glass is not luminous, is that beautiful wall of cup is thin, transparent, lamp has the noctilucence effect under shining.Imitative in recent years beautiful product constantly occurs on market, also constantly improves to some extent qualitatively.Mostly be to be that main raw material is made with macromolecular material.For make the technology for producing artificial jadeware product on weight and texture near natural jade, add stone flour therein.Zhejiang Province refreshing carving company adds embedded photoluminescent material and makes the imitative jade carving arts (ZL92105254.2 with noctilucence effect, ZL93110823.1, ZL931009227.2 etc.) have much ornamental value, yet these imitative beautiful products are that macromolecular material is polymerized, on hardness, rigidity, feel, still have the vestige of plastics, not ideal enough on the emulation degree.Chinese patent (publication number) CN1186789A has described a kind of synthetic jewel and manufacture method thereof, and its raw material is general expression MNAl 2-xB xO 4The sintered body of expression constitutes, and M represents alkaline-earth metal in the formula, and N represents rare earth element, 0.1≤x≤1.Its synthesis temperature is 1550-1700 ℃, and pressure is 2 above normal atmosphere, is two steps to burn till (the first step synthesis material), and the material of its description is not fully aware of, the synthesis temperature height, and raw material variety is single, and the luminous gem of making can not reach the performance of its description.
Summary of the invention
The objective of the invention is to adopt Inorganic Chemicals, by practical and advanced sintering process, synthetic at a lower temperature performance is more near natural jade, and after illumination, can send the artificial jade of twilight sunset, its quality densification, exquisiteness, tough and tensile, hardness are 3-7, and density is 2.5-4.6g/cm 3
Concrete scheme of the present invention is:
1, luminous jade chemical constitution expression of the present invention is:
AM β bM ' β cSiO 2DAl 2O 3EEu 2O 3FB 2O 3GLn 2O 3HZrO 2Wherein: M is the combination of one or more elements among Ca, Sr, Ba, Mg, Zn, the Cd;
M ' is the combination of one or more elements among Be, Mg, Zn, the Cd;
β is the combination of one or both elements among O, the S;
Ln is the combination of one or more elements among Ce, Pr, La, Dy, Ho, Nd, Er, Bi, Ga, Sb, Lu, Y, Mn, Mo, Cr, Sn, Cu, the Tm;
A, b, c, d, e, f, g, h are respectively mole coefficients, 0.6≤a≤6; 0≤b≤4; 0.037≤c≤3; 0.01≤d≤8; 0.00001≤e≤0.15; 0≤f≤0.4; 0＜g≤0.2; 0≤h≤0.3.
2, as 1 described artificial luminescent jade, its chemical constitution expression is:
aMO·bM′O·cSiO 2·dAl 2O 3·e Eu 2O 3·fB 2O 3·gLn 2O 3·hZrO 2
1.5≤a≤3.5 wherein; 0.5≤b≤1.5; 1.5≤c≤2.5; 0.01≤d≤0.4, the orchid, blue green, green, Yellow luminous that can realize jade.
3,, it is characterized in that its chemical constitution expression is as 1 described artificial luminescent jade:
aMO·cSiO 2·dAl 2O 3·eEu 2O 3·fB 2O 3·gLn 2O 3·hZrO 2
0.6≤a≤1.4 wherein; B=0; 0.037≤c≤0.3; 0.7≤d≤1.3; 0≤f≤0.1 can realize that yellow-green colour is luminous.
4, as 1 described artificial luminescent jade, the expression of its chemical constitution is:
aMO·c SiO 2·dAl 2O 3·eEu 2O 3·fB 2O 3·gLn 2O 3·hZrO 2
3.4≤a≤4.6 wherein; B=0; 0.037≤c≤0.4; 6.5 blue green emitting can be realized in≤d≤7.5.
In the above-mentioned chemical constitution expression formula, when a, b, c, the variation of d value, M, M ', the element of β representative and the difference of element combinations, it is luminous to make jade produce different colours.If: 1.5≤a≤3.5,0.5≤b≤1.5,1.5≤c≤2.5,0.01≤d≤0.4, β is an oxygen element, it is blue, blue green, green, Yellow luminous that jade is produced; At this moment, if M is Sr, M ' is Mg, and the main chemical constitution composition that changes jewel according to a value is Sr 2MgSi 2O 7Or Sr 3MgSi 2O 8If M is Sr, the Ca element of different ratios, can realize that then orchid is green, green, Yellow luminous, the main chemical constitution composition of jade is (SrCa) 2MgSi 2O 7Or (SrCa) 3MgSi 2O 8If 0.6≤a≤1.4,0≤b≤0.1,0.037≤c≤0.3,0.7≤d≤1.3, β is an oxygen element, and M is the Sr element, and it is luminous to make jade produce yellow-green colour, and the main chemical constitution composition of jade is SrAl 2O 4If M is the Ca element, also can realize blue violet light, the main chemical constitution composition of jade is CaAl 2O 4If 3.4≤a≤4.6,0≤b≤0.1,0.037≤c≤0.4,6.5≤d≤7.5, β is an oxygen element, and M is the Sr element, can make jade produce blue green emitting, the main chemical constitution composition of jade Sr 4Al 14O 25If 0.5≤a≤1.5,0≤b≤0.2,0.037≤c≤0.1,0.01≤d≤0.1, β is an element sulphur, and M is that Ca can realize emitting red light, and main chemical constitution composition is CaS.
Experiment showed, that the adding of Zr element can increase the hardness of jade, the variation of Al, Si amount of element has tangible influence to density, chemical stability, the machining property (as intensity etc.) of jade.
Raw materials used during products production of the present invention is the oxide compound, oxyhydroxide, carbonate, sulfide etc. of above-mentioned element; Luminescent materials such as also available different kinds of ions activated aluminate, silicate, sulfide.Calculate the raw material consumption by required element proportioning, mix, moulding, high-temperature pressure or pressurization, the one or many sintering forms.Its concrete steps are:
If adopt disposable burning till, the ratio weighing contains the raw material of above-mentioned element on request, and after mixing, water or binding agent are piled up or compression moulding, after the oven dry, adopts gradually and heats up, and under reducing atmosphere, generally adopts H 2, H 2+ N 2Or CO was in 1100-1550 ℃ of sintering 0.5-24 hour; Maybe will contain the raw material weighing in proportion of above-mentioned element, mix, in hot pressing furnace or under the hot isostatic pressing furnace reduction atmosphere, generally adopt H 2, H 2+ N 2Or CO is under 600-1450 ℃, hot pressed sintering 0.5-4 hour, and pressure 5-300MPa.
If adopt twice firing, after will containing the raw material of above-mentioned element weighing mixing in proportion, in stove under 800-1550 ℃, elder generation's pre-burning 1-20 hour, with burned material grind, sieve back water or binding agent is piled up or compression moulding heats up gradually, under 1000-1550 ℃ in reducing atmosphere, as H 2, H 2+ N 2Or CO sintering 0.5-10 hour; Maybe will contain above-mentioned element raw material weighing in proportion, mix after, in stove under 800-1550 ℃, first pre-burning 1-20 hour, with burned material grind, sieve the back in heat (waiting quiet) is pressed stove in reducing atmosphere, as H 2, H 2+ N 2Or CO pressed sintering 0.5-4 hour in 600-1450 ℃ of heat (waiting quiet), pressure 5-300MPa;
Certainly, can also be with the raw material that contains above-mentioned element after weighing mixes in proportion, in stove 800-1300 ℃, first pre-burning 10-40 hour, in reducing atmosphere, produce monocrystalline with conventional crystal pulling method or zone melting method again, produce jewel truly.
The manufacture method of this luminous jade can be by following scheme implementation:
1, the manufacture method of the described artificial luminescent jade of above-mentioned 1-4, be that ratio by the requirement of chemical constitution expression formula will contain the raw materials of compound of required element after grinding, mixing, moulding, under reducing atmosphere, through 600-1550 ℃, under the 0-400MPa pressure, carry out once or double sintering 0.5-30h forms; The oxide compound that the described raw materials of compound that contains required element is this element, oxyhydroxide, carbonate, sulfide etc.
2, as the manufacture method of artificial luminescent jade as described in 1, the described raw materials of compound that contains required element can be different kinds of ions activated aluminate, silicate or sulfide luminescent material and Al 2O 3, SiO 2, ZrO 2Or contain the compound of this oxide compound; Three kinds of oxide compounds can use wherein one or more; Its usage quantity is that the weight percent that accounts for luminescent material is:
Al 2O 3 0-10％
SiO 2 0-8％
ZrO 2 0-5％
And its consumption sum is not more than 10%.
3, as the manufacture method of 1 described artificial luminescent jade, be the raw material that ratio weighing on request contains above-mentioned element, after mixing, water or binding agent are piled up or compression moulding, after the oven dry, adopt gradually and heat up, and under reducing atmosphere, generally adopt H 2, H 2+ N 2Or CO was in 1100-1550 ℃ of sintering 0.5-24 hour.
4, as the manufacture method of artificial luminescent jade as described in 1, be to contain the raw material weighing in proportion of above-mentioned element, to mix, under hot pressing or hot isostatic pressing furnace reduction atmosphere, generally adopt H 2, H 2+ N 2Or CO is under 600-1450 ℃, hot pressing or HIP sintering 0.5-4 hour, and pressure 5-300MPa.
5, as the manufacture method of artificial luminescent jade as described in 1, be the raw material weighing in proportion that will contain above-mentioned element, mix after, in stove 800-1550 ℃, elder generation's pre-burning 1-20 hour, with burned material grinding, sieve back water or binding agent accumulation or compression moulding, heat up gradually, under 1000-1550 ℃, in reducing atmosphere, as H 2, H 2+ N 2Or CO sintering 0.5-10 hour
6, as the manufacture method of artificial luminescent jade as described in 1, be the raw material weighing in proportion that will contain above-mentioned element, mix after, in stove 800-1550 ℃, select pre-burning 1-20 hour, with burned material grind, sieve the back in hot pressing or static pressure stove in reducing atmosphere, as H 2, H 2+ N 2Or CO is in 600-1450 ℃ of hot pressing or HIP sintering 0.1-4 hour, pressure 5-300MPa.
7, as the manufacture method of artificial luminescent jade as described in 1, be the raw material weighing in proportion that will contain above-mentioned element, mix after, in stove 800-1200 ℃, first pre-burning 10-40 hour, under reducing atmosphere, produce monocrystalline with conventional crystal pulling method or zone melting method again.
This jade of making, hardness are between the 3-7 degree, and density is 2.5-4.6g/cm 3, its quality densification, exquisiteness, tough and tensile are as then moistening more smooth, bright and clean through polishing.In the dark can be luminous after illumination, according to the difference of combination of materials, can present 1-100 hour afterglow.Luminous afterglow intensity testing method is the thin slice that the luminous jade that will make is polished into 10mm, in the darkroom, deposit more than 10 hours, taking-up places standard D65 light source under 1000LX illumination, and irradiation 10min tries its time dependent luminous intensity with the glorious degrees instrumentation.
The present invention compared with prior art because jade of the present invention is to form with the inorganic raw material sintering, more near natural jade, the while has more luminous after illumination on its quality and the sense organ, makes the luminous jade of multiple color.
Embodiment
Example 1 Yellow luminous jade
Choose a=2.0, b=1.1, c=1.8, d=0.01, e=0.03, f=0.1, g=0.05, h=0, M=Sr 0.05Ca 0.95, M '=Mg 0.95Zn 0.05, β=0
Ln＝Dy 0.95Sb 0.05
Raw material Molecular weight Mol ratio Weight (g)
SrCO 3 147.62 2.0×0.05 14.76
CaCO 3 100.0 2.0×0.95 190.00
MgO 40.31 1.1×0.95 42.12
ZnO 81.31 1.1×0.05 4.47
SiO 2 60.09 1.8×1.0 108.16
Al 2O 3 102.0 0.01×1.0 1.02
Eu 2O 3 352 0.03×1.0 10.56
B 2O 3 69.62 0.1×1.0 6.96
Dy 2O 3 374 0.05×0.95 17.77
Sb 2O 3 291.6 0.05×0.05 0.73
Above-mentioned raw materials being weighed by weight, behind the porphyrize mixing, under 10MPa pressure, be pressed into right cylinder, be encased in the plasticity-mould, through the further compacting of 200MPa isostatic cool pressing, is 90%N in atmosphere 2+ 10%H 2The reducing atmosphere stove in, be warming up to 1150 ℃ gradually, constant temperature was reduced to room temperature gradually and is promptly got Yellow luminous artificial luminescent jade after 5 hour.
Example 2 blue look luminous jades
Choose a=2.2, b=1.0, c=2.0, d=0.04, e=0.03, f=0.05, g=0.03, h=0.01, M=Sr 0.95Ca 0.05, M '=Mg, Ln=Dy 0.90Bi 0.10, β=0
Raw material Molecular weight Mol ratio Weight (g)
SrO 103.62 2.2×0.95 216.57
CaO 56.08 2.2×0.05 6.17
MgO 40.31 1.0×1.0 40.31
SiO 2 60 2.0×1.0 120
Al 2O 3 102.0 0.04×1.0 4.08
Eu 2O 3 352 0.03×1.0 10.56
B 2O 3 69.62 0.05×1.0 3.48
Dy 2O 3 374 0.03×0.9 10.10
Bi 2O 3 466 0.03×0.1 1.4
ZrO 2 123.22 0.01×1.0 1.23
Above-mentioned raw materials is weighed by weight, behind the porphyrize mixing, be encased in the hot pressing furnace mould, the ventilation atmosphere is 95%N 2+ 5%H 2Reducing atmosphere, heat up gradually and be forced into 1000 ℃, under the 30MPa, sintering 1 hour is reduced to the artificial luminescent jade that room temperature promptly gets luminous blue look gradually.
Example 3 avy blue luminous jades
Choose a=3.2, b=0.8, c=2.0, d=0, e=0.01, f=0.05, g=0.03, h=0, M=Sr, M '=Mg, Ln=Nd 0.95La 0.05, β=0
Raw material Molecular weight Mol ratio Weight (g)
SrO 103.62 3.2×1.0 331.58
MgO 40.31 0.8×1.0 32.25
SiO 2 60 2.0×1.0 120
Eu 2O 3 352 0.01×1.0 3.52
B 2O 3 69.62 0.05×1.0 3.48
Nd 2O 3 336.4 0.03×0.95 9.59
La 2O 3 325.8 0.03×0.05 0.49
Above-mentioned raw materials is weighed by weight, behind the porphyrize mixing, at logical H 2High Temperature Furnaces Heating Apparatus in 1300 ℃ of first sintering 4 hours, after the cooling with block sintered compact porphyrize, after crossing 400 eye mesh screens, with the aqueous solution that adds CMC the powder that sieves is compacted into definite shape, after the oven dry, in the High Temperature Furnaces Heating Apparatus of logical N2, be warming up to 1420 ℃ gradually, behind the constant temperature 5 hours, reduce to the artificial luminescent jade that room temperature promptly gets luminous avy blue gradually.
Example 4 blue green emitting jades
Choose a=4.0, b=0.05, c=0, d=7.0, e=0.01, f=0.03, g=0.01, h=0.05, M=Sr 0.85Ca 0.15, M '=Zn, Ln=Dy 0.9La 0.1, β=0
Raw material Molecular weight Mol ratio Weight (g)
SrO 103.62 4.0×0.85 352.31
CaO 56.08 4.0×0.15 33.65
ZnO 81.31 0.05×1.0 4.07
Al 2O 3 102 7.0×1.0 714
Eu 2O 3 352 0.01×1.0 3.52
B 2O 3 69.62 0.03×1.0 2.09
Dy 2O 3 374 0.01×0.9 3.37
La 2O 3 325.8 0.01×0.1 0.33
ZrO 2 123.22 0.05×1.0 6.16
Above-mentioned raw materials is weighed by weight, behind the porphyrize mixing, at logical N 2In the High Temperature Furnaces Heating Apparatus of+CO in 1450 ℃ of sintering 4 hours, after the cooling with block sintered compact porphyrize, after crossing 300 eye mesh screens, screen underflow is put into the hot pressing furnace mould, under N2 atmosphere, heat up gradually and be forced into 1200 ℃, be incubated 2 hours, pressure 30MPa reduces to room temperature gradually and promptly gets luminous blue green artificial luminescent jade.
Example 5 blue violet light jades
Choose a=1.0, b=0, c=0, d=1.0, e=0.01, f=0.01, g=0.02, h=0, M=Ca, Ln=Nd 0.5Tm 0.5, β=0
Raw material Molecular weight Mol ratio Weight (g)
CaCO 3 100.0 1.0×1.0 100.00
Al 2O 3 102.0 1.0×1.0 102
Eu 2O 3 352 0.01×1.0 3.52
B 2O 3 69.62 0.01×1.0 0.7
Nd 2O 3 336.4 0.02×0.5 3.36
Tm 2O 3 385.8 0.02×0.5 3.86
Above-mentioned raw materials is weighed by weight, behind the porphyrize mixing, in air,, behind the porphyrize, adopt zone melting method, at 96%Ar+4%H in 1100 ℃ of calcinings 30 hours 2Generate the long monocrystalline of about 10mm under the atmosphere.
Example 6 yellow-green colour luminous jades
Choose a=1.0, b=0, c=0.037, d=1.01, e=0.01, f=0.03, g=0.01, h=0.008, M=Sr, Ln=Dy 0.95Y 0.05, β=0
Raw material Molecular weight Mol ratio Weight (g)
A SrO 103.62 1.0×1.0 103.62
Al 2O 3 102.0 1.0×1.0 102
Eu 2O 3 352 0.01×1.0 3.52
B 2O 3 69.62 0.03×1.0 2.09
Dy 2O 3 374 0.01×0.95 3.55
Y 2O 3 225.82 0.01×0.05 0.11
B Kaolin 2.0
ZrO 2 1.0
Feldspar 2.0
Accurately take by weighing the category-A raw material by weight, behind the porphyrize mixing, at logical 90%N 2+ 10%H 2High Temperature Furnaces Heating Apparatus in, in 1350 ℃ of sintering 4 hours, after the cooling,, cross 300 mesh sieves with block sintered compact porphyrize, add less water mixing porphyrize with the category-B material that accurately takes by weighing, be molded into definite shape, dry back is at reducing atmosphere (90%N 2+ 10%H 2) in the stove, slowly be warming up to 1400 ℃, be incubated 4 hours, reduce to room temperature gradually and promptly get luminous yellowish green artificial luminescent jade.
The performance of above-mentioned example is listed in table 1
Table 1:
Main chemical composition Hardness Proportion Luminous afterglow intensity (mcd/m 2) Fluorescent lifetime (min)
10(min) 30(min) 60(min) 90(min)
Example 1 Ca 2MgSi 2O 7 6.5 3.2 200 66 30 16 630
Example 2 Sr 2MgSi 2O 7 6.2 3.1 210 77 40 25 1875
Example 3 Sr 3MgSi 2O 7 6.3 3.1 100 35 18 10 1230
Example 4 Sr 4Al 14O 25 6.2 3.6 598 222 117 77 5940
Example 5 CaAl 14O 25 7.1 3.6 46 16 8 5 362
Example 6 SrAl 2O 4 6.9 3.5 625 239 123 84 4756
Annotate: fluorescent lifetime is the minimum visible diopter 0.32mcd/m of specimen intelligent eye 2Time

Claims (4)

1, a kind of artificial luminescent jade is characterized in that sending twilight sunset after the illumination, and hardness is 3-7, and density is 2.5-4.6g/cm 3The chemical constitution expression formula is:
aMβ·bM′β·cSiO 2·dAl 2O 3·eEu 2O 3·fB 2O 3·gLn 2O 3·hZrO 2
Wherein: M is the combination of one or more elements among Ca, Sr, Ba, Mg, Zn, the Cd;
M ' is the combination of one or more elements among Be, Mg, Zn, the Cd;
β is the combination of one or both elements among O, the S;
Ln be a kind of among Ce, Pr, La, Dy, Ho, Nd, Er, Bi, Ga, Sb, Lu, Y, Mn, Mo, Cr, Sn, Cu, the Tm or
The combination of multiple element;
A, b, c, d, e, f, g, h are respectively mole coefficients,
0.6≤a≤6；0≤b≤4；0.037≤c≤3；
0.01≤d≤8；0.00001≤e≤0.15；
0≤f≤0.4；0＜g≤0.2；0≤h≤0.3。
2, artificial luminescent jade as claimed in claim 1 is characterized in that the chemical constitution expression is:
aMO·bM′O·cSiO 2·dAl 2O 3·eEu 2O 3·fB 2O 3·gLn 2O 3·hZrO 2
1.5≤a≤3.5 wherein; 0.5≤b≤1.5; 1.5≤c≤2.5; 0.01≤d≤0.4.
3, artificial luminescent jade as claimed in claim 1 is characterized in that the chemical constitution expression is:
aMO·cSiO 2·dAl 2O 3·eEu 2O 3·fB 2O 3·gLn 2O 3·hZrO 2
0.6≤a≤1.4 wherein; B=0; 0.037≤c≤0.3; 0.7≤d≤1.3; 0≤f≤0.1.
4, artificial luminescent jade as claimed in claim 1 is characterized in that the expression of chemical constitution is:
aMO·cSiO 2·dAl 2O 3·eEu 2O 3·fB 2O 3·gLn 2O 3·hZrO 2
3.4≤a≤4.6 wherein; B=0; 0.037≤c≤0.4; 6.5≤d≤7.5.
CNB99126777XA 1999-04-09 1999-11-13 Luminous jade and preparing process thereof Expired - Fee Related CN1192077C (en)

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CN1325603C (en) * 2003-11-27 2007-07-11 上海交通大学 Long-time afterglow luminescent silicate material and its producing method
CN102442816B (en) * 2011-10-17 2013-12-18 王蕴渔 Synthetic grey-white jade and manufacturing method thereof
CN104086155B (en) * 2013-07-05 2016-08-24 孟庆洪 Artificial colour jade material, its production method and application
CN104802278B (en) * 2015-04-07 2018-01-12 浙江省地质矿产研究所 Method for preparing jade article by adopting 3D printing technology
CN106116537B (en) * 2016-06-24 2019-01-11 保磁（广州）磁性材料有限公司 Ceramic lapis lazuli, the powder for being used to prepare ceramic lapis lazuli and its preparation and application
CN106010522A (en) * 2016-06-28 2016-10-12 东台市天源荧光材料有限公司 Dysprosium ion-doped borosilicate red nano fluorescent powder and preparation method thereof

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