CN103910491A - Lead-containing sealing glass powder having selective spectrum absorption characteristic, and manufacturing method thereof - Google Patents

Lead-containing sealing glass powder having selective spectrum absorption characteristic, and manufacturing method thereof Download PDF

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Publication number
CN103910491A
CN103910491A CN201310003969.XA CN201310003969A CN103910491A CN 103910491 A CN103910491 A CN 103910491A CN 201310003969 A CN201310003969 A CN 201310003969A CN 103910491 A CN103910491 A CN 103910491A
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glass powder
oxide
compound
sealing
absorption characteristic
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CN103910491B (en
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黄幼榕
李要辉
王晋珍
汪洪
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BEIJING HANGBO NEW MATERIAL TECHNOLOGY Co Ltd
China Building Materials Academy CBMA
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BEIJING HANGBO NEW MATERIAL TECHNOLOGY Co Ltd
China Building Materials Academy CBMA
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Abstract

The present invention discloses lead-containing sealing glass powder having a selective spectrum absorption characteristic, and a preparation method thereof, wherein a lead-containing low temperature sealing glass system is adopted as a base component, and is added with a rare earth oxide capable of making the sealing glass produce the selective spectrum absorption characteristic and a transition metal oxide, and the weight percentage ratio of the total amount of the base component to the total amount of the rare earth oxide and the transition metal oxide in the lead-containing sealing glass is 100:0.12-10.0. The lead-containing sealing glass powder prepared according to the method has the selective spectrum absorption characteristic, is applicable for the light radiation heating sealing processes adopting ultraviolet light, visible light or infrared light as the heating source, can be used for insulating sealing or air tightness sealing of electrical vacuum devices, electronic components or vacuum insulating glasses, and has advantages of low sealing temperature, good chemical stability, appropriate expansion coefficient, easy preparation, continuous large-scale industrial production and the like.

Description

There is leaded sealing glass powder and the manufacture method thereof of spectral selectivity absorption characteristic
Technical field
The present invention relates to field of glass production technology, particularly a kind of leaded sealing glass powder and manufacture method thereof with spectral selectivity absorption characteristic.
Background technology
Electronic devices and components, electron tube or vacuum subassembly often adopt leaded sealing glass powder to make insulated enclosure or Leakless sealing, and conventionally using electrical heating element as thermal source, heat transmission is take convection current as main.There is the shortcomings such as heat-up time is long, sealing-in process is slow, it is high to consume energy, production efficiency is low in the method, is particularly needed entirety to be heated to glass powder sealing temperature by sealing-in object and just can complete sealing-in, and it is restricted in some applications.For example: OLED indicating meter needs to use sealing glass powder to form Leakless sealing during fabrication between two substrates, approximately 400 ~ 450 ℃ of sealing temperatures.But the pixel region apart from the substrate sealed portion distance of positions from approximately 80 ~ 90 millimeters, in sealing-in process, temperature must not exceed 80 ℃, therefore adopts the traditional heating method for sealing will be due to the overheated performance degradation that causes.For another example: the sealing-in heat-processed of toughened vacuum glass, as adopted traditional heating method for sealing that the stress that makes toughened glass is removed, cannot keep tempering intensity.
Optical radiation heating is another kind of conventional type of heating, has that heating efficiency is high, speed fast, be easy to the advantages such as control.Particularly can utilize the difference of differing materials optical absorptive character, realize being heated up by the selectivity of sealing-in object different sites.If sealing glass powder much larger than by sealing-in object body, may be significantly less than sealing-in place by the bulk temperature of sealing-in object, the injury of having avoided high temperature to bring to the absorption that adds thermo-optical in the time of sealing-in.Therefore be applied in above two examples, optical radiation heating, compared with electrical heating element heating, has outstanding advantage.Optical radiation heating can adopt laser apparatus or spot light lamp as thermal source, as: visible laser (420 or 640 nanometer), infrared light laser apparatus (810 nanometer), ultraviolet laser (355 nanometer), infrared lamp (810 ~ 5000 nanometer) etc.The key that realizes selective local heating is to use the suitable sealing glass powder with spectral selectivity absorption characteristic, and the optical radiation heating source matching with it, so that absorbing radiation energy effectively.
Existing leaded low meiting sealing frils meets traditional electrical heating element entirety, and to add heat sealing mode be that object designs, and the emphasis of concern concentrates on the sealing temperature of glass powder, thermal expansivity, mobility, sealing strength, insulation resistance and chemical stability etc.While using it for optical radiation heating sealing process, be prone to that rate of heating is slow, heating region large, by series of problems such as sealing-in object bulk temperature risings.
Summary of the invention
The object of the embodiment of the present invention is the defect for above-mentioned prior art, provide one to there is spectral selectivity absorption characteristic, can be used for optical radiation selectivity heating sealing process, and sealing temperature is low, chemical stability is good, the coefficient of expansion is suitable, is easy to the leaded sealing glass powder of preparation.
Another object of the present invention is to provide a kind of method for the manufacture of above-mentioned leaded sealing glass powder, the method not only makes the manufacturing processed of sealing glass powder be easy to carry out, and can be according to different characteristic requirements, add rare earth oxide and the transition metal oxide of different components, the requirement of the sealing-in that meets electron tube, electronic devices and components, vacuum subassembly to glass light spectral property, melting temperature sealing, the coefficient of expansion.
The technical scheme that the present invention takes is to achieve these goals:
A kind of leaded sealing glass powder with spectral selectivity absorption characteristic, take leaded low temperature sealing glass system as basic components, in described basic components, be added with rare earth oxide and the transition metal oxide that can make seal glass produce spectral selectivity absorption characteristic.
It is that leaded low temperature sealing glass and phosphorus are leaded low temperature sealing glass that described basic components is selected from bismuth, wherein:
Described basic components is that low temperature sealing glass forms by lead, and described lead is the component that leaded low temperature sealing glass comprises following weight part: PbO30.0 ~ 87.0 part, B 2o 35.0 ~ 30.0 parts, ZnO0 ~ 20.0 part, SiO 20.2 ~ 5.0 part of Al 2o 30.2 ~ 5.0 part,, Bi 2o 30 ~ 10.0 part, P 2o 50 ~ 5.0 part, K 2o0 ~ 0.5 part, Na 2o0 ~ 0.5 part, Li 2o0 ~ 0.5 part, MgO0 ~ 0.5 part, CaO0 ~ 0.5 part, SrO0 ~ 2.0 part, BaO0 ~ 2.0 part, SnO0 ~ 6.0 part, Sn 2o0 ~ 2.0 part, TeO 20 ~ 3.0 part, V 2o 50 ~ 2.0 part, Sb 2o 30 ~ 2.0 part, Ag 2o0 ~ 10.0 part, PbF 20 ~ 10.0 part.
Described rare earth oxide and transition metal oxide are selected from: cerium oxide, ferric oxide, chromium sesquioxide, nickel sesquioxide, cobalt sesquioxide, cupric oxide, iron protoxide, Vanadium Pentoxide in FLAKES and Manganse Dioxide; The weight part of each component is: CeO 20 ~ 2.0 part, Fe 2o 30.02~2.0 part, Cr 2o 30.02 ~ 2.0 part, Co 2o 30.02 ~ 2.0 part, CuO0.02 ~ 4.0 part, FeO0.02 ~ 4.0 part, Ni 2o 30.02~2.0 part, V 2o 50 ~ 1.0 part, MnO0 ~ 1.0 part.
Weight ratio between the gross weight of described basic components and described rare earth oxide and the gross weight of transition metal oxide is 100:0.12~10.0.
The present invention also provides the method for utilizing the above-mentioned leaded sealing glass powder with spectral selectivity absorption characteristic to prepare glass powder, comprises the following steps:
Step 101: according to the composition of described basic components and described rare earth oxide and transition metal oxide, take the compound that various oxide raw materials and/or oxide compound are corresponding, fully mix, make compound; The weight part of the compound that described oxide compound is corresponding is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 0.5~3 hour at 800~1200 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound obtaining in step 102 is cured cooling, grinds to form host glass powder;
Step 104: choose or prepare the coefficient of expansion for (100~96) × 10 -7/ ℃ fire resistant infilling;
Step 105: the fire resistant infilling that the host glass powder that step 103 is obtained and step 4 obtain fully mixes.
Another kind provided by the invention utilizes the above-mentioned leaded sealing glass powder with spectral selectivity absorption characteristic to prepare the method for glass powder, comprises the following steps:
Step 101: according to the composition of described basic components, take various oxide compounds and/or compound corresponding to oxide compound in described basic components, fully mix, make compound; The weight part of the compound that described oxide compound is corresponding is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 0.5~3 hour at 800~1200 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound that step 102 is obtained is cured cooling, grinds to form host glass powder;
Step 104: choose rare earth oxide and the transition metal oxide that can make sealing glass powder produce characteristic spectrum absorption characteristic, through being fully mixed and made into mixture;
Step 105: choose or prepare the coefficient of expansion for (100~96) × 10 -7/ ℃ fire resistant infilling;
Step 106: the fire resistant infilling obtaining in the mixture obtaining in the host glass powder obtaining in step 103, step 104 and step 105 is fully mixed.
The cumulative volume sum of the mixture obtaining in the host glass powder obtaining in described step 103 and step 104 and the volume ratio of described fire resistant infilling are: 100:5~25.
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is:
The leaded sealing glass powder that adopts the method for invention to prepare, has spectral selectivity absorption characteristic, can be used for optical radiation heating sealing process; Meanwhile, seal glass also has that sealing temperature is low, chemical stability good, the coefficient of expansion is suitable, is easy to preparation, can realizes the advantage of the large-scale industrial production of serialization.Be applicable to the optical radiation heating sealing technology of electronic devices and components, electron tube and vacuum glass.
Accompanying drawing explanation
Fig. 1 is the schema of the manufacture method of a kind of leaded sealing glass powder with spectral selectivity absorption characteristic that the embodiment of the present invention provides;
Fig. 2 is the schema that another kind that the embodiment of the present invention provides has the manufacture method of the leaded sealing glass powder of spectral selectivity absorption characteristic.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
Referring to Fig. 1, leaded low meiting sealing frils raw material of the present invention is made up of industrial chemicals or raw mineral materials, comprise: plumbous oxide, boric acid, zinc oxide, bismuthous oxide bismuth trioxide, Vanadium Pentoxide in FLAKES, silicon-dioxide, aluminum oxide, salt of wormwood, soda ash, Quilonum Retard, magnesium oxide, calcium carbonate, Strontium carbonate powder, barium carbonate, tin protoxide (II), tindioxide (IV), tellurium dioxide, Vanadium Pentoxide in FLAKES, antimonous oxide, Silver Nitrate, plumbous fluoride, cerium dioxide, ferric oxide, chromium sesquioxide, nickel sesquioxide, cobalt sesquioxide, cupric oxide, iron protoxide, Vanadium Pentoxide in FLAKES and Manganse Dioxide.These raw materials are converted into corresponding ratio of weight and number according to its oxide content and prepare burden, take the basic components and rare earth oxide, the transition metal oxide that can produce selective spectral absorption characteristic of leaded low temperature sealing glass, mix, again through high temperature melting, cooling, pulverize, grind, sieve, make host glass powder, also can add the fire resistant infilling with the specific coefficient of expansion, host glass powder and fire resistant infilling are evenly mixed, make the leaded low meiting sealing frils with spectral selectivity absorption characteristic.
Referring to Fig. 2, another kind of preparation method provided by the invention, first weighing: the basic components that takes leaded low temperature sealing glass, mix, again through high temperature melting, cooling, pulverize, grind, sieve, host glass powder processed, weigh again rare earth oxide and the transition metal oxide that can produce selective spectral absorption characteristic, choose or prepare the fire resistant infilling with the specific coefficient of expansion, host glass powder, rare earth oxide and transition metal oxide and fire resistant infilling are evenly mixed, make the leaded low meiting sealing frils with spectral selectivity absorption characteristic.
Be described further in conjunction with specific embodiments with regard to the processing request of leaded sealing glass powder performance index and product below.
Embodiment 1
A kind of manufacture method of the leaded sealing glass powder with spectral selectivity absorption characteristic:
Step 101: according to the component of 1 correspondence of embodiment in table 1, i.e. the composition of basic components and rare earth oxide and transition metal oxide, takes the compound that various oxide raw materials and/or oxide compound are corresponding, fully mixes, and makes compound; Wherein, boron oxide, calcium oxide, strontium oxide, barium oxide and silver suboxide are selected its corresponding compound, and the weight part of corresponding compound is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 3 hours at 1200 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound obtaining in step 102 is cooling on iron plate, cooled glass fragment is pulverized, ground, cross 200 mesh sieves, obtain host glass powder;
Host glass powder composed as follows (gram):
PbO30.0,B 2O 330.0,ZnO20.0,P 2O 55.0,SiO 25.0,Al 2O 35.0,MgO0.5,CaO0.5,SrO2.0,BaO2.0。
Wherein also comprise rare earth oxide and the transition metal oxide that can make seal glass produce spectral selectivity absorption characteristic, it is composed as follows (gram):
CeO 20.3,Fe 2O 30.3,Cr 2O 30.3,Ni 2O 30.3,Co 2O 30.4,CuO4.0,FeO4.0,V 2O 50.2,MnO0.2。
Wherein, the weight ratio between the gross weight of basic components and described rare earth oxide and the gross weight of transition metal oxide is: 100:10.0.
Step 104: preparation fire resistant infilling;
The preparation process of fused silica powder filler is: adopt three classes or four quartz-like glass to be greater than 300 mesh sieves through pulverizing, grind, crossing, can make low-expansion coefficient fused silica powder filler.
Step 105: the fire resistant infilling obtaining in the host glass powder obtaining in step 103 and step 104 is fully mixed;
Host glass powder and fused silica powder are 100:5 according to volume ratio, fully mix, and make the barium crown sealed glass powder of the present embodiment.
The leaded sealing glass powder of the present embodiment is that the coefficient of expansion is 86.8 × 10 -7/ ℃, melting temperature sealing is the leaded sealing by fusing glass powder of 520 ℃.This leaded sealing glass powder has lower thermal expansivity and moderate melting temperature sealing, and has suction infrared spectral characteristic, and can be used for heated light sources is the optical radiation heating sealing process of infrared laser or infrared lamp (wavelength 810 ~ 5000 nanometers).
Embodiment 2
A kind of manufacture method of the leaded sealing glass powder with spectral selectivity absorption characteristic:
Step 101: according to the component of 2 correspondences of embodiment in table 1, i.e. the composition of basic components and rare earth oxide and transition metal oxide, takes the compound that various oxide raw materials and/or oxide compound are corresponding, fully mixes, and makes compound; Make compound; Wherein, boron oxide, potassium oxide, sodium oxide, Lithium Oxide 98min and silver suboxide are selected its corresponding compound, and the weight part of corresponding compound is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 0.5 hour at 800 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound that step 102 is obtained is cooling on iron plate, pulverizes cooled glass fragment, grind, and crosses 300 mesh sieves, obtains host glass powder;
The host glass powder processing composed as follows (gram):
PbO87.0,B 2O 35.0,Bi 2O 31.0,P 2O 51.0,SiO 20.5,Al 2O 30.5,K 2O0.5,Na 2O0.5,Li 2O0.5,SnO0.5,SnO 20.5,TeO 20.5,V 2O 50.5Sb 2O 30.5,Ag 2O,PbF 20.5。
Wherein also comprise rare earth oxide and the transition metal oxide that can make seal glass produce spectral selectivity absorption characteristic, it is composed as follows (gram):
CeO 22.0,Fe 2O 32.0,Cr 2O 32.0,Ni 2O 30.2,Co 2O 30.1,CuO0.1,FeO0.5,V 2O 50.1,MnO0.1。
Wherein, the weight ratio between the gross weight of basic components and described rare earth oxide and the gross weight of transition metal oxide is: 100:7.1.
Step 104: preparation fire resistant infilling;
Fire resistant infilling was the calcium metatitanic acid lead powder of 300 mesh sieves
Step 105: the host glass powder obtaining in step 103 is fully mixed with the calcium lead titanate filler obtaining in step 104;
Host glass powder is that 100:10 fully mixes with calcium metatitanic acid lead powder according to volume ratio, makes the barium crown sealed glass powder of the present embodiment.
The leaded sealing glass powder coefficient of expansion of the present embodiment is 91.6 × 10 -7/ ℃, melting temperature sealing is 430 ℃, has lower melting temperature sealing and good fluidity, and UV-light is had to selective spectral absorption characteristic, can be used for heated light sources is the optical radiation heating sealing process of ultraviolet laser or ultraviolet lamp (wavelength 355 nanometers).
Embodiment 3
A kind of manufacture method of the leaded sealing glass powder with spectral selectivity absorption characteristic:
Step 101: according to the component of 3 correspondences of embodiment in table 1, i.e. the composition of basic components and rare earth oxide and transition metal oxide, takes the compound that various oxide raw materials and/or oxide compound are corresponding, fully mixes, and makes compound; Wherein, boron oxide, calcium oxide, strontium oxide, barium oxide and silver suboxide are selected its corresponding compound, and the weight part of corresponding compound is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 2 hours at 1100 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound that step 102 is obtained is cooling on iron plate, pulverizes cooled glass fragment, grind, and crosses 300 mesh sieves, obtains host glass powder;
The host glass powder processing composed as follows (gram):
PbO46.0,B 2O 36.0,ZnO1.3,Bi 2O 310.0,SiO 20.2,Al 2O 30.2,K 2O0.2,Na 2O0.1,Li 2O0.2,MgO0.2,CaO0.2,SrO0.2,BaO0.2,SnO6.0,SnO 22.0,TeO 23.0,V 2O 52.0,Sb 2O 32.0,Ag 2O10.0,PbF 210.0。
Step 104: choose rare earth oxide and the transition metal oxide that can make sealing glass powder produce characteristic spectrum absorption characteristic, i.e. the transition metal oxide of embodiment 3 in table 1, through being fully mixed and made into mixture;
Compositions of mixtures following (gram):
Fe 2O 30.02,Cr 2O 30.02,Ni 2O 30.02,Co 2O 30.02,CuO0.02,FeO0.02。
Step 105: choose fire resistant infilling;
Fire resistant infilling was the beta-eucryptite of 300 mesh sieves;
Step 106: the beta-eucryptite powder obtaining in the mixture obtaining in the host glass powder obtaining in step 103, step 104 and step 105 is fully mixed;
Wherein, the proportionlity of various powders is as follows:
The host glass powder obtaining in step 103: the weight percent=100:0.12 of the mixture obtaining in step 104;
The mixture cumulative volume sum obtaining in the host glass powder obtaining in step 103 and step 104: the volume ratio=100:15 of the fire resistant infilling obtaining in step 105.
Fully be mixed and made into the leaded sealing glass powder of the present embodiment.
The leaded sealing glass powder coefficient of expansion of the present embodiment is 81.2 × 10 -7/ ℃, melting temperature sealing is 460 ℃, has lower melting temperature sealing and good fluidity, and visible ray is had to selective spectral absorption characteristic, can be used for heated light sources is the optical radiation heating sealing process of visible laser (wavelength 380 ~ 780 nanometers).
Embodiment 4
A kind of manufacture method of the leaded sealing glass powder with spectral selectivity absorption characteristic:
Step 101: according to the component of 4 correspondences of embodiment in table 1, i.e. the composition of basic components, takes the compound that various oxide raw materials and/or oxide compound are corresponding, fully mixes, and makes compound; Wherein, boron oxide and silver suboxide are selected its corresponding compound, and the weight part of corresponding compound is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 1 hour at 1000 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound that step 102 is obtained is cooling on iron plate, pulverizes cooled glass fragment, grind, and crosses 300 mesh sieves, obtains host glass powder;
(%) composed as follows of the host glass powder processing:
PbO62.9,B 2O 39.1,ZnO1.0,Bi 2O 35.0,P 2O 53.1,SiO 21.4,Al 2O 32.4,TeO 22.0,V 2O 51.0,Sb 2O 31.0,Ag 2O5.5,PbF 25.5。
Step 104: choose rare earth oxide and the transition metal oxide that can make sealing glass powder produce characteristic spectrum absorption characteristic, in table 1 in the second component rare earth oxide and transition metal oxide, through being fully mixed and made into mixture;
Mixture has following composition:
CeO 20.1,Fe 2O 30.2,Cr 2O 30.2,Ni 2O 32.0,Co 2O 32.0,CuO1.0,FeO1.0,V 2O 51.0,MnO1.0。
Step 105: choose fire resistant infilling;
Fire resistant infilling was the trichroite powder of 300 mesh sieves;
Step 106: the trichroite powder obtaining in the mixture obtaining in the glass powder obtaining in step 103, step 104 and step 105 is fully mixed;
Wherein, the proportionlity of various powders is as follows:
The weight percent of the mixture obtaining in the host glass powder obtaining in step 103 and step 104 is: 100:8.5; The volume ratio of the fire resistant infilling obtaining in the cumulative volume sum of the mixture that the host glass powder obtaining in step 103 and step 104 obtain and step 105 is: 100:25.
Fully be mixed and made into the leaded sealing glass powder of the present embodiment.
The leaded sealing glass powder coefficient of expansion of the present embodiment is 79.1 × 10 -7/ ℃, melting temperature sealing is 500 ℃, have lower melting temperature sealing and good fluidity, infrared light is had to selective spectral absorption characteristic, can be used for heated light sources is the optical radiation heating sealing process of infrared laser or infrared lamp (wavelength 810 ~ 5000 nanometers).
Step 104: choose fire resistant infilling;
Fire resistant infilling was the trichroite powder of 300 mesh sieves;
Composition and the performance of three kinds of embodiment seal glasses of table 1
Table 1 has been summed up embodiment mono-, embodiment bis-, embodiment tri-and embodiment tetra-totally four kinds of different componentss and have the low temperature leaded sealing glass powder of different spectral selectivity absorption characteristics, the coefficient of expansion, melting temperature sealing and volume specific resistance.
Beneficial effect of the present invention is: the present invention can realize the adjustment to glass powder spectral selectivity absorption characteristic by the component of adjusting glass, can adapt to the needs of different optical radiation heated light sources; Meanwhile, by adjusting kind and the content of fire resistant infilling, realize the coefficient of expansion to leaded seal glass, the adjustment of sealing by fusing working temperature, thereby complete difference by the sealing-in of seal, sealing materials (as: glass, pottery or metal).
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (8)

1. one kind has the leaded sealing glass powder of spectral selectivity absorption characteristic, it is characterized in that, take leaded low temperature sealing glass system as basic components, in described basic components, be added with rare earth oxide and the transition metal oxide that can make seal glass produce spectral selectivity absorption characteristic.
2. the leaded sealing glass powder with spectral selectivity absorption characteristic according to claim 1, it is characterized in that, described basic components is that low temperature sealing glass forms by lead, and described lead is 30.0 ~ 87.0 parts of the component that leaded low temperature sealing glass comprises following weight part: PbO, B 2o 35.0 ~ 30.0 parts, 0 ~ 20.0 part of ZnO, Bi 2o 30 ~ 10.0 part, P 2o 50 ~ 5.0 part, SiO 20.2 ~ 5.0 part of Al 2o 30.2 ~ 5.0 part, K 20 ~ 0.5 part of O, Na 2o0 ~ 0.5 part, Li 20 ~ 0.5 part of O, 0 ~ 0.5 part of MgO, 0 ~ 0.5 part of CaO, 0 ~ 2.0 part of SrO, 0 ~ 2.0 part of BaO, 0 ~ 6.0 part of SnO, Sn 20 ~ 2.0 part of O, TeO 20 ~ 3.0 part, V 2o 50 ~ 2.0 part, Sb 2o 30 ~ 2.0 part, Ag 2o0 ~ 10.0 part, PbF 20 ~ 10.0 part.
3. the leaded sealing glass powder with spectral selectivity absorption characteristic according to claim 3, it is characterized in that, described rare earth oxide and transition metal oxide are selected from: cerium oxide, ferric oxide, chromium sesquioxide, nickel sesquioxide, cobalt sesquioxide, cupric oxide, iron protoxide, Vanadium Pentoxide in FLAKES and Manganse Dioxide; The weight part of each component is: CeO 20 ~ 2.0 part, Fe 2o 30.02~2.0 part, Cr 2o 30.02 ~ 2.0 part, Ni 2o 30.02~2.0 part, Co 2o 30.02 ~ 2.0 part, CuO0.02 ~ 4.0 part, 0.02 ~ 4.0 part of FeO, V 2o 50 ~ 1.0 part, 0 ~ 1.0 part of MnO.
4. there is according to claim 3 the leaded sealing glass powder of spectral selectivity absorption characteristic, it is characterized in that, the weight ratio between the gross weight of described basic components and described rare earth oxide and the gross weight of transition metal oxide is 100:0.12~10.0.
5. utilize the leaded sealing glass powder with spectral selectivity absorption characteristic described in claim 4 to prepare the method for glass powder, it is characterized in that, comprise the following steps:
Step 101: according to the composition of described basic components and described rare earth oxide and transition metal oxide, take the compound that various oxide raw materials and/or oxide compound are corresponding, fully mix, make compound; The weight part of the compound that described oxide compound is corresponding is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 0.5~3 hour at 800~1200 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound obtaining in step 102 is cured cooling, grinds to form host glass powder;
Step 104: choose or prepare the coefficient of expansion for (100~96) × 10 -7/ ℃ fire resistant infilling;
Step 105: the fire resistant infilling that the host glass powder that step 103 is obtained and step 104 obtain fully mixes.
6. preparation method according to claim 5, is characterized in that, the volume ratio of described host glass powder and described fire resistant infilling is: 100:5-25.
7. utilize the leaded sealing glass powder with spectral selectivity absorption characteristic described in claim 1 to prepare the method for glass powder, it is characterized in that, comprise the following steps:
Step 101: according to the composition of described basic components, take various oxide compounds and/or compound corresponding to oxide compound in described basic components, fully mix, make compound; The weight part of the compound that described oxide compound is corresponding is the corresponding parts by weight that are converted into according to its oxide content;
Step 102: the compound obtaining in step 101 is melted 0.5~3 hour at 800~1200 ℃, obtain the melt liquid of compound;
Step 103: the melt liquid of the compound that step 102 is obtained is cured cooling, grinds to form host glass powder;
Step 104: choose rare earth oxide and the transition metal oxide that can make sealing glass powder produce characteristic spectrum absorption characteristic, through being fully mixed and made into mixture;
Step 105: choose or prepare the coefficient of expansion for (100~96) × 10 -7/ ℃ fire resistant infilling;
Step 106: the mixture obtaining in the host glass powder obtaining in step 103, step 104 and the fire resistant infilling of step 105 gained are fully mixed.
8. preparation method according to claim 7, is characterized in that, the cumulative volume sum of the mixture obtaining in described host glass powder and step 104 and the volume ratio of described fire resistant infilling are: 100:5~25.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104682909A (en) * 2015-02-11 2015-06-03 福建省南平市三金电子有限公司 Novel crystal oscillator low-temperature glass packaging structure and packaging technology thereof
CN106495488A (en) * 2016-11-03 2017-03-15 常州市鼎日环保科技有限公司 A kind of preparation method of electro permanent magnetic high-purity sealing glass material
CN107399908A (en) * 2017-08-21 2017-11-28 北京工业大学 A kind of photo-thermal heat absorbing glass sealing-in material and preparation method thereof
CN107540229A (en) * 2017-09-05 2018-01-05 珠海彩珠实业有限公司 A kind of toughened vacuum glass glass powder with low melting point and preparation method thereof
CN112299720A (en) * 2020-11-16 2021-02-02 成都光明光电有限责任公司 Low temperature sealing glass

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3973975A (en) * 1972-04-21 1976-08-10 Owens-Illinois, Inc. PbO-containing sealing glass with higher oxide of a cation to avoid PbO reduction
CN1214355A (en) * 1997-10-14 1999-04-21 旭硝子株式会社 Hermetic sealing composition
CN1798708A (en) * 2003-04-16 2006-07-05 康宁股份有限公司 Hermetically sealed glass package and method of fabrication
CN1915877A (en) * 2006-09-11 2007-02-21 中国建筑材料科学研究总院 Rare earth elements doped sealing by fusing glass powder without lead, and manufacturing method
CN101103429A (en) * 2004-10-13 2008-01-09 康宁股份有限公司 Hermetically sealed glass package and method of fabrication
CN101139165A (en) * 2006-08-18 2008-03-12 康宁股份有限公司 Boro-silicate glass frits for hermetic sealing of light emitting device displays
CN102120693A (en) * 2010-01-11 2011-07-13 上海歌灵新材料科技有限公司 Lead-free sealing glass and preparation method thereof
CN102471137A (en) * 2009-07-31 2012-05-23 旭硝子株式会社 Sealing glass, sealing material and sealing material paste for semiconductor devices, and semiconductor device and process for production thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3973975A (en) * 1972-04-21 1976-08-10 Owens-Illinois, Inc. PbO-containing sealing glass with higher oxide of a cation to avoid PbO reduction
CN1214355A (en) * 1997-10-14 1999-04-21 旭硝子株式会社 Hermetic sealing composition
CN1798708A (en) * 2003-04-16 2006-07-05 康宁股份有限公司 Hermetically sealed glass package and method of fabrication
CN101103429A (en) * 2004-10-13 2008-01-09 康宁股份有限公司 Hermetically sealed glass package and method of fabrication
CN101139165A (en) * 2006-08-18 2008-03-12 康宁股份有限公司 Boro-silicate glass frits for hermetic sealing of light emitting device displays
CN1915877A (en) * 2006-09-11 2007-02-21 中国建筑材料科学研究总院 Rare earth elements doped sealing by fusing glass powder without lead, and manufacturing method
CN102471137A (en) * 2009-07-31 2012-05-23 旭硝子株式会社 Sealing glass, sealing material and sealing material paste for semiconductor devices, and semiconductor device and process for production thereof
CN102120693A (en) * 2010-01-11 2011-07-13 上海歌灵新材料科技有限公司 Lead-free sealing glass and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104682909A (en) * 2015-02-11 2015-06-03 福建省南平市三金电子有限公司 Novel crystal oscillator low-temperature glass packaging structure and packaging technology thereof
CN106495488A (en) * 2016-11-03 2017-03-15 常州市鼎日环保科技有限公司 A kind of preparation method of electro permanent magnetic high-purity sealing glass material
CN106495488B (en) * 2016-11-03 2019-04-30 桐乡市振业玻璃有限公司 A kind of preparation method of electromagnetically sealing glass material
CN107399908A (en) * 2017-08-21 2017-11-28 北京工业大学 A kind of photo-thermal heat absorbing glass sealing-in material and preparation method thereof
CN107540229A (en) * 2017-09-05 2018-01-05 珠海彩珠实业有限公司 A kind of toughened vacuum glass glass powder with low melting point and preparation method thereof
CN112299720A (en) * 2020-11-16 2021-02-02 成都光明光电有限责任公司 Low temperature sealing glass
CN112299720B (en) * 2020-11-16 2022-04-12 成都光明光电有限责任公司 Low temperature sealing glass

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