CN103910490A - Lead-free sealing glass powder having selective spectrum absorption characteristic, and manufacturing method thereof - Google Patents
Lead-free sealing glass powder having selective spectrum absorption characteristic, and manufacturing method thereof Download PDFInfo
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Abstract
The present invention discloses lead-free sealing glass powder having a selective spectrum absorption characteristic, and a preparation method thereof, wherein a lead-free 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-free sealing glass is 100:0.1-20.0. The lead-free 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
Technical field
The present invention relates to field of glass production technology, particularly a kind of barium crown sealed glass powder and manufacture method thereof with spectral selectivity absorption characteristic.
Background technology
Electronic devices and components, electron tube or vacuum subassembly often adopt barium crown sealed glass powder to make insulated enclosure or Leakless sealing, and conventionally using electrical heating element as thermal source, heat transmission is taking 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 DEG C 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 DEG C, 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 lead-free low-temperature sealing glass powder 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 barium crown sealed glass powder of preparation.
Another object of the present invention is to provide a kind of method for the manufacture of above-mentioned barium crown sealed 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 barium crown sealed glass powder with spectral selectivity absorption characteristic, taking lead-free low-temperature seal 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 lead-free low-temperature seal glass that described basic components is selected from bismuth, wherein:
Described bismuth is the component that lead-free low-temperature seal glass comprises following weight part: Bi
2o
330.0 ~ 96.0 parts, ZnO2.0 ~ 20.0 part, B
2o
32.0 ~ 20.0 parts, Al
2o
30 ~ 3.0 part, SiO
20 ~ 3.0 part, Li
2o0 ~ 2.0 part, Na
2o0 ~ 2.0 part, K
2o0 ~ 2.0 part, BaO0 ~ 5.0 part, MgO0 ~ 1.0 part, CaO0 ~ 1.0 part, SrO0 ~ 2.0 part, SnO0 ~ 3.0 part, SnO
20 ~ 1.0 part, TiO
20 ~ 2.0 part, CuO0 ~ 2.0 part, Sb
2o
30 ~ 2.0 part, P
2o
50 ~ 2.0 part, V
2o
50 ~ 1.0 part, Ag
2o0 ~ 2.0 part;
Described rare earth oxide and the transition metal oxide that makes seal glass produce spectral selectivity absorption characteristic is selected from cerium oxide, ferric oxide, iron protoxide, chromium sesquioxide, cobalt sesquioxide, nickel sesquioxide, cupric oxide, Vanadium Pentoxide in FLAKES and Manganse Dioxide, and the parts by weight of each component are: CeO
20 ~ 5.0 part, Cr
2o
30.02 ~ 2.0 part, FeO0 ~ 5.0 part, Fe
2o
30.02～5.0 part, Co
2o
30.02 ~ 3.0 part, CuO0 ~ 5.0 part, Ni
2o
30.02～3.0 part, V
2o
50 ~ 2.0 part, MnO0 ~ 2.0 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 100:0.1～20.0.
The present invention also provides the method for utilizing the above-mentioned barium crown sealed 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 DEG C, 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 (80 ~ 96) × 10
-7/ DEG C 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.
The volume ratio of described host glass powder and described fire resistant infilling is: 100:5 ~ 25.
Another kind provided by the invention utilizes the above-mentioned barium crown sealed 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 DEG C, 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 (80～96) × 10
-7/ DEG C 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 described host glass powder 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 barium crown sealed glass powder that adopts the method for invention to prepare, there is spectral selectivity absorption characteristic, being applicable to heating source is that sealing process is heated in ultraviolet, optical radiation visible or infrared light, can be used for electron tube, electronic devices and components or vacuum glass insulated enclosure or Leakless sealing; 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.
Brief description of the drawings
Fig. 1 is the schema of the manufacture method of a kind of barium crown sealed 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 barium crown sealed 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, lead-free low-temperature seal glass powder raw material of the present invention is made up of industrial chemicals or raw mineral materials, comprise: bismuthous oxide bismuth trioxide, Vanadium Pentoxide in FLAKES, boric acid, aluminum oxide, zinc oxide, antimonous oxide, silicon-dioxide, Quilonum Retard, soda ash, salt of wormwood, magnesium oxide, calcium carbonate, Strontium carbonate powder, barium carbonate, tin protoxide (II), tindioxide (IV), Vanadium Pentoxide in FLAKES, titanium dioxide, Silver Nitrate, cerium dioxide, chromium sesquioxide, iron protoxide, ferric oxide, cupric oxide, nickel sesquioxide, cobalt sesquioxide, 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 lead-free low-temperature seal glass, mix, again through high temperature melting, cooling, pulverize, grind, sieve, host glass powder processed, 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 lead-free low-temperature sealing glass powder 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 lead-free low-temperature seal 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 lead-free low-temperature sealing glass powder with spectral selectivity absorption characteristic.
Be described further in conjunction with specific embodiments with regard to the processing request of barium crown sealed glass powder performance index and product below.
Embodiment 1
A kind of manufacture method of the barium crown sealed glass powder with spectral selectivity absorption characteristic:
Step 101: according to the composition of embodiment in table 11, 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, Lithium Oxide 98min, potassium oxide, sodium 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 DEG C, 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, its coefficient of expansion is 98.0 × 10
-7/ DEG C:
Host glass powder composed as follows (gram):
Bi
2O
330．0，ZnO20．0，B
2O
320．0，A1
2O
33．0，SiO
23．0，Li
2O2．0，K
2O2．0，Na
2O2．0，MgO1．0,CaO1．0，SrO2．0，BaO5．0，TiO
22．0,CuO2．0,V
2O
51．0，SnO3．0，SnO
21．0，Ag
2O2．0。
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
20．5，Fe
2O
30．5,Cr
2O
32．0,Ni
2O
33．0,CoO3．0,CuO5．0,FeO5．0．MnO
21．0。
Step 104: preparation fire resistant infilling;
The preparation process of 13 1 eucryptite fillers is: adopt Quilonum Retard, aluminum oxide and opticglass quartz sand according to Li
2o:A1
2o
3: SiO
2chemical formula calculated mass, than batching, mixes, and fires 5 hours, then pass through crushing grinding at 1250 DEG C, crosses 300 mesh sieves and can make 13 1 eucryptite fillers, and the coefficient of expansion of 13 1 eucryptite fillers is one 51 × 10
-7/ DEG C.
Step 105: the fire resistant infilling that the host glass powder that step 1O3 is obtained and step 104 obtain fully mixes;
Be that 100:5 fully mix with 13 1 eucryptite powder fillers according to volume ratio by host glass powder, make the barium crown sealed glass powder of the present embodiment.
The barium crown sealed glass powder of the present embodiment is that the coefficient of expansion is 90.8 × 10
-7/ DEG C, melting temperature sealing is the sealing by fusing glass powder without lead of 505 DEG C.This barium crown sealed glass powder 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 barium crown sealed glass powder with spectral selectivity absorption characteristic:
Step 101: according to the second component 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, Lithium Oxide 98min, potassium oxide, sodium 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 1 hour at 900 DEG C, 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, its coefficient of expansion is 102.0 × 10
-7/ DEG C;
Host glass powder composed as follows (gram):
Bi
2O
370.0，ZnO13.0，B
2O
311.0，Al
2O
31.0,SiO
20.5,Li
2O0.2，K
2O0.1，Na
2O0.1，MgO0.1,CaO0.1SrO0.5，BaO2.0，TiO
20.2,CuO0.6,Sb
2O
30.3，P
2O
52.0，V
2O
50.1,SnO0.5,SnO
20.1,Ag
2O0.1。
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
25.0，Fe
2O
35.0,Cr
2O
30.1,NiO0.2,CoO0.1,FeO0.5,V
2O
52.0,MnO
22.0。
Step 104: choose fire resistant infilling;
Fire resistant infilling was the fused silica powder of 300 mesh sieves;
Step 105: the glass powder obtaining in step 103 is fully mixed with the fused silica powder obtaining in step 104;
Host glass powder and fused silica powder are that to be fully mixed and made into the coefficient of expansion be 82.7 × 10 to 100:25 according to volume ratio
-7/ DEG C barium crown sealed glass powder.
The present embodiment barium crown sealed glass powder coefficient of expansion is 82.7 × 10
-7/ DEG C, melting temperature sealing is 465 DEG C.The melting temperature sealing of this glass is lower and mobility is better, and UV-light is had to selective spectral absorption characteristic, and 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 barium crown sealed glass powder with spectral selectivity absorption characteristic:
Step 101: according to the component of embodiment in table 13, 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 is 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; Take the compound that various oxide raw materials and/or oxide compound are corresponding, fully mix, make compound;
Step 102: the compound obtaining in step 101 is melted 0.5 hour at 800 DEG C, 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;
Host glass powder composed as follows (gram):
Bi
2O
396.0，B
2O
32.0，ZnO2.0。
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，NiO0.02，Co
2O
30.02，FeO0.02。
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 host glass powder obtaining in step 103: the weight percent=100:0.1 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 barium crown sealed glass powder coefficient of expansion of the present embodiment is 93.8 × 10
-7/ DEG C, melting temperature sealing is 455 DEG C.The melting temperature sealing of this glass is lower and mobility is better, and visible ray is had to selective spectral absorption characteristic, and 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 barium crown sealed glass powder with spectral selectivity absorption characteristic:
Step 101: according to the component of embodiment in table 14, 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, the weight part of boron oxide, Lithium Oxide 98min, potassium oxide, sodium oxide, calcium oxide, strontium oxide, barium oxide, compound that silver suboxide is corresponding is the corresponding parts by weight that are converted into according to its oxide content; Take the compound that various oxide raw materials and/or oxide compound are corresponding, fully mix, make compound;
Step 102: the compound obtaining in step 101 is melted 2 hours at 1200 DEG C, 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;
Host glass powder composed as follows (gram):
Bi
2O
375.3，ZnO15.2，B
2O
34.6，Al
2O
30.4,SiO
21.3,Li
2O0.1，K
2O0.1，Na
2O0.1，MgO0.4,CaO0.3SrO0.5，BaO1.0，TiO
20.1,Sb
2O
32.0，P
2O
50.3，V
2O
50.1，SnO0.3,SnO
20.1,Ag
2O0.1。
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 4 in table 1, through being fully mixed and made into mixture;
Compositions of mixtures following (gram):
CeO
20.1，Fe
2O
30.2，Cr
2O
30.2，NiO0.5，CoO0.8，FeO2.5，V
2O
51.0，MnO
20.5。
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 host glass powder obtaining in step 103: the weight percent=100:5.8 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=100:18 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 barium crown sealed glass powder coefficient of expansion of the present embodiment is 89.0 × 10
-7/ DEG C, melting temperature sealing is 460 DEG C.The melting temperature sealing of this glass is lower and mobility is better, and infrared light is had to selective spectral absorption 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).
The bismuth that table 1 has a spectral selectivity absorption characteristic is that each component concentration of barium crown sealed glass powder is as follows:
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 leadless sealed 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 barium crown sealed 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 amendment 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 barium crown sealed glass powder of spectral selectivity absorption characteristic, it is characterized in that, taking lead-free low-temperature seal 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 barium crown sealed glass powder with spectral selectivity absorption characteristic according to claim 1, is characterized in that, it is lead-free low-temperature seal glass that described basic components is selected from bismuth, wherein:
Described bismuth is the component that lead-free low-temperature seal glass comprises following weight part: Bi
2o
330.0 ~ 96.0 parts, ZnO2.0 ~ 20.0 part, B
2o
32.0 ~ 20.0 parts, Al
2o
30 ~ 3.0 part, SiO
20 ~ 3.0 part, Li
2o0 ~ 2.0 part, Na
2o0 ~ 2.0 part, K
2o0 ~ 2.0 part, BaO0 ~ 5.0 part, MgO0 ~ 1.0 part, CaO0 ~ 1.0 part, SrO0 ~ 2.0 part, SnO0 ~ 3.0 part, SnO
20 ~ 1.0 part, TiO
20 ~ 2.0 part, CuO0 ~ 2.0 part, Sb
2o
30 ~ 2.0 part, P
2o
50 ~ 2.0 part, V
2o
50 ~ 1.0 part, Ag
2o0 ~ 2.0 part.
3. the barium crown sealed glass powder with spectral selectivity absorption characteristic according to claim 1, it is characterized in that, described rare earth oxide and the transition metal oxide that makes seal glass produce spectral selectivity absorption characteristic is selected from cerium oxide, ferric oxide, iron protoxide, chromium sesquioxide, cobalt sesquioxide, nickel sesquioxide, cupric oxide, Vanadium Pentoxide in FLAKES and Manganse Dioxide, and the parts by weight of each component are: CeO
20 ~ 5.0 part, Cr
2o
30.02 ~ 2.0 part, FeO0 ~ 5.0 part, Fe
2o
30.02～5.0 part, Co
2o
30.02 ~ 3.0 part, CuO0 ~ 5.0 part, Ni
2o
30.02～3.0 part, V
2o
50 ~ 2.0 part, MnO0 ~ 2.0 part.
4. the barium crown sealed glass powder according to claim 3 with spectral selectivity absorption characteristic, 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 100:0.1～20.0.
5. utilize the barium crown sealed 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 DEG C, 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 (180～150) × 10
-7/ DEG C 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.
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 barium crown sealed 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 DEG C, 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 (80～96) × 10
-7/ DEG C 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310003905.XA CN103910490B (en) | 2013-01-07 | There is barium crown sealed glass powder and the manufacture method thereof of spectral selection absorption characteristic |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310003905.XA CN103910490B (en) | 2013-01-07 | There is barium crown sealed glass powder and the manufacture method thereof of spectral selection absorption characteristic |
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| Publication Number | Publication Date |
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| CN103910490A true CN103910490A (en) | 2014-07-09 |
| CN103910490B CN103910490B (en) | 2016-11-30 |
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| 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 |
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| CN107840575A (en) * | 2017-11-29 | 2018-03-27 | 苏州福莱威封装技术有限公司 | A kind of glass powder with low melting point and preparation method thereof |
| CN108033684A (en) * | 2017-12-13 | 2018-05-15 | 海南中航特玻科技有限公司 | A kind of back of the body silver glass powder used for solar batteries and preparation method |
| CN113149445A (en) * | 2021-02-01 | 2021-07-23 | 上海大学 | Method for uniformly refining low-temperature lead-free glass powder by using ultrahigh-pressure microjet and application thereof |
| CN113299422A (en) * | 2021-05-07 | 2021-08-24 | 江西师范大学 | Crystalline silicon solar cell front silver paste and preparation method thereof |
| CN114212995A (en) * | 2021-12-27 | 2022-03-22 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method suitable for OLED sealing solder |
| CN114212995B (en) * | 2021-12-27 | 2023-10-20 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of OLED sealing solder |
| CN116675435A (en) * | 2023-05-17 | 2023-09-01 | 武汉理工大学 | Glass powder, laser sealing glass slurry, vacuum glass and sealing process thereof |
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