CN103910491B - There is leaded sealing glass powder and the manufacture method thereof of spectral selection absorption characteristic - Google Patents

There is leaded sealing glass powder and the manufacture method thereof of spectral selection absorption characteristic Download PDF

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CN103910491B
CN103910491B CN201310003969.XA CN201310003969A CN103910491B CN 103910491 B CN103910491 B CN 103910491B CN 201310003969 A CN201310003969 A CN 201310003969A CN 103910491 B CN103910491 B CN 103910491B
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oxide
leaded
glass powder
sealing
compound
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CN103910491A (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 invention discloses a kind of leaded sealing glass powder with spectral selection absorption characteristic and preparation method thereof, component based on leaded low temperature sealing glass system, added with rare earth oxide and the transition metal oxide that seal glass can be made to produce spectral selection absorption characteristic in described basic components.In described leaded seal glass, weight fraction between basic components total amount and described rare earth and transition metal oxide total amount is than for 100:0.12 ~ 10.0.The leaded sealing glass powder prepared according to the method for the invention, there is spectral selection absorption characteristic, being applicable to heating source is ultraviolet, the visible or light radiation heating process for sealing of 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, it is easy to preparation, can realize the advantage such as large-scale industrial production of serialization.

Description

There is leaded sealing glass powder and the manufacture method thereof of spectral selection absorption characteristic
Technical field
The present invention relates to field of glass production technology, particularly to a kind of, there is spectral selection absorption characteristic Leaded sealing glass powder and manufacture method thereof.
Background technology
Electronic devices and components, electron tube or vacuum subassembly are close through making insulation frequently with leaded sealing glass powder Envelope or Leakless sealing, generally transmit based on convection current using heating as thermal source, heat.The method is deposited Heat time heating time length, the shortcoming such as sealing-in process is slow, power consumption is high, production efficiency is low, particularly by sealing-in object Needs are integrally heated glass dust sealing temperature just can complete sealing-in so that it is be restricted in some applications. Such as: OLED display needs to use sealing glass powder to form Leakless sealing between two pieces of substrates during fabrication, Sealing temperature about 400~450 DEG C.But away from the substrate sealed portion distance of positions from the pixel region of about 80~90 millimeters, During sealing-in, temperature must not exceed 80 DEG C, and therefore employing traditional heating method for sealing will be owing to crossing thermally-induced property Can decay.For another example: the sealing-in heating process of toughened vacuum glass, as used traditional heating method for sealing to make The stress of safety glass is removed, it is impossible to keep tempering intensity.
Light radiation heating is another kind of conventional mode of heating, has that the efficiency of heating surface is high, speed is fast, be prone to control The advantages such as system.Particularly may utilize the difference of different materials optical absorptive character, it is achieved to by sealing-in object not Heat up with the selectivity at position.If the absorption of heating light is much larger than by sealing-in object body by sealing glass powder, May be significantly less than at sealing-in by the bulk temperature of sealing-in object when sealing-in, it is to avoid the injury that high temperature brings. Therefore being applied in above two examples, light radiation heating, compared with heating heating, has outstanding advantage. Light radiation heating can use laser instrument or spotlight as thermal source, such as: (420 or 640 receive visible laser Rice), infrared light laser instrument (810 nanometer), ultraviolet laser (355 nanometer), infrared lamp (810~5000 Nanometer) etc..Realizing it is critical only that of selective local heating uses the suitable spectral selection that has to absorb The sealing glass powder of characteristic, and matched light radiation heating source, in order to effectively absorb emittance.
Existing leaded low meiting sealing frils is to meet traditional heating entirety and add heat sealing mode to be Purpose and design, concern focus on the sealing temperature of glass dust, thermal coefficient of expansion, mobility, Sealing strength, insulation resistance and chemical stability etc..When using it for light radiation heating process for sealing, easily go out Existing firing rate is slow, heating region big, risen high series of problems by sealing-in object bulk temperature.
Summary of the invention
The purpose of the embodiment of the present invention is the defect for above-mentioned prior art, it is provided that one has optical electivity Property absorption characteristic, can be used for light radiation selectivity heating process for sealing, and sealing temperature is low, chemical stability Well, the coefficient of expansion is suitable, it is easy to the leaded sealing glass powder of preparation.
Another object of the present invention is to provide a kind of method for manufacturing above-mentioned leaded sealing glass powder, should Method not only makes the manufacture process of sealing glass powder be prone to carry out, and can according to different characteristic requirements, Add the rare earth oxide of different component and transition metal oxide, meet electron tube, electronic devices and components, The sealing-in of vacuum subassembly is to glass light spectral property, melting temperature sealing, the requirement of the coefficient of expansion.
The present invention adopts the technical scheme that to achieve these goals:
A kind of leaded sealing glass powder with spectral selection absorption characteristic, with leaded low temperature sealing glass system Component based on system, added with seal glass can be made to produce spectral selection absorption characteristic in described basic components Rare earth oxide and transition metal oxide.
Described basic components is selected from the leaded low temperature sealing glass of the leaded low temperature sealing glass of bismuth system and phosphorus system, wherein:
Described basic components is made up of lead system low temperature sealing glass, and the leaded low temperature sealing glass of described lead system includes The component of following weight portion: PbO 30.0~87.0 parts, B2O35.0~30.0 parts, ZnO 0~20.0 parts, SiO2 0.2~5.0 part, Al2O30.2~5.0 part, Bi2O30~10.0 part, P2O50~5.0 part, K2O 0~0.5 part, Na2O 0~0.5 part, Li2O 0~0.5 part, MgO 0~0.5 part, CaO 0~0.5 part, SrO 0~2.0 parts, BaO 0~2.0 Part, SnO 0~6.0 parts, SnO20~2.0 part, TeO20~3.0 part, V2O50~2.0 part, Sb2O30~2.0 part, Ag2O 0~10.0 part, PbF20~10.0 part.
Described rare earth oxide and transition metal oxide by cerium oxide, iron sesquioxide, chromic oxide, Nickel sesquioxide, cobalt sesquioxide, copper oxide, ferrous oxide, vanadic anhydride and manganese oxide composition;Respectively The weight portion of component is: CeO20~2.0 part, Fe2O30.02~2.0 part, Cr2O30.02~2.0 part, Co2O3 0.02~2.0 part, CuO 0.02~4.0 parts, FeO 0.02~4.0 parts, Ni2O30.02~2.0 part, V2O50~1.0 part, MnO 0~1.0 parts.
Between gross weight and described rare earth oxide and the gross weight of transition metal oxide of described basic components Weight ratio be 100:0.12~10.0.
The present invention also provides for utilizing the above-mentioned leaded sealing glass powder with spectral selection absorption characteristic to prepare The method of glass dust, comprises the following steps:
Step 101: according to described basic components and described rare earth oxide and the composition of transition metal oxide, Weigh various oxide raw material and/or compound corresponding to oxide, be sufficiently mixed, make compound;Institute The weight portion stating compound corresponding to oxide is the corresponding weight portion being converted into according to its oxide content Number;
Step 102: the compound obtained 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 obtained in step 102 is carried out solidification cooling, grinds to form base Matter glass dust;
Step 104: choose or prepare the coefficient of expansion for (-100~96) × 10-7/ DEG C fire resistant infilling;
Step 105: the fire resistant infilling that host glass powder step 103 obtained and step 4 obtain is sufficiently mixed Uniformly.
The another kind that the present invention provides utilizes the above-mentioned leaded seal glass with spectral selection absorption characteristic Powder prepares the method for glass dust, comprises the following steps:
Step 101: according to the composition of described basic components, weigh the various oxides in described basic components and / or compound corresponding to oxide, it is sufficiently mixed, makes compound;The compound that described oxide is corresponding Weight portion be the corresponding parts by weight being converted into according to its oxide content;
Step 102: the compound obtained 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 compound step 102 obtained carries out solidification cooling, grinds to form substrate Glass dust;
Step 104: choose rare earth oxide and the transition that sealing glass powder can be made to produce characteristic spectrum absorption characteristic Metal-oxide, is adequately mixed and makes mixture;
Step 105: choose or prepare the coefficient of expansion for (-100~96) × 10-7/ DEG C fire resistant infilling;
Step 106: by the mixture obtained in the host glass powder obtained by step 103, step 104 and The fire resistant infilling obtained in step 105 carries out being sufficiently mixed uniformly.
The cumulative volume of the mixture obtained in host glass powder obtained in described step 103 and step 104 Sum with the volume ratio of described fire resistant infilling is: 100:5~25.
The technical scheme that the embodiment of the present invention provides has the benefit that
The leaded sealing glass powder using the method for invention to prepare, has spectral selection absorption characteristic, available Process for sealing is heated in light radiation;Meanwhile, seal glass also have that sealing temperature is low, chemical stability good, The coefficient of expansion is suitable, it is easy to preparation, the advantage that can realize the large-scale industrial production of serialization.It is suitable for Sealing technology is heated in light radiation in electronic devices and components, electron tube and vacuum glass.
Accompanying drawing explanation
Fig. 1 is a kind of leaded seal glass with spectral selection absorption characteristic that the embodiment of the present invention provides The flow chart of the manufacture method of powder;
Fig. 2 be the embodiment of the present invention provide another kind have spectral selection absorption characteristic containing leaded joint glass The flow chart of the manufacture method of glass powder.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to the present invention Embodiment is described in further detail.
Seeing Fig. 1, the leaded low meiting sealing frils raw material of the present invention is made up of industrial chemicals or raw mineral materials, Including: lead oxide, boric acid, zinc oxide, bismuth oxide, phosphorus pentoxide, silicon dioxide, aluminium oxide, Potassium carbonate, soda, lithium carbonate, magnesium oxide, calcium carbonate, strontium carbonate, brium carbonate, Tin monoxide (II), Tin ash (IV), tellurium dioxide, vanadic anhydride, antimony oxide, silver nitrate, Lead difluoride, dioxy Change cerium, iron sesquioxide, chromic oxide, nickel sesquioxide, cobalt sesquioxide, copper oxide, oxidation Asia Ferrum, vanadic anhydride and manganese oxide.These raw materials are converted into corresponding parts by weight according to its oxide content Ratio carries out dispensing, weighs the basic components of leaded low temperature sealing glass and can produce selective spectral absorption characteristic Rare earth oxide, transition metal oxide, mixing, then through high temperature melting, cool down, pulverize, grind, Sieve, make host glass powder, also can add the fire resistant infilling with the specific coefficient of expansion, by host glass Powder and fire resistant infilling uniformly mix, and make the leaded low meiting sealing frils with spectral selection absorption characteristic.
See Fig. 2, the another kind of preparation method that the present invention provides, first weighing: weigh leaded low temperature sealing glass Basic components, mixing, then through high temperature melting, cool down, pulverize, grind, sieve, host glass processed Powder, then weigh rare earth oxide and the transition metal oxide that can produce selective spectral absorption characteristic, choose Or preparation has the fire resistant infilling of the specific coefficient of expansion, by host glass powder, rare earth oxide and transition metal Oxide and fire resistant infilling uniformly mix, and make the leaded low-temperature sealing glass with spectral selection absorption characteristic Glass powder.
Below the processing request with regard to leaded sealing glass powder performance indications and product make in conjunction with specific embodiments into One step explanation.
Embodiment 1
A kind of manufacture method of the leaded sealing glass powder with spectral selection absorption characteristic:
Step 101: according to the component of embodiment 1 correspondence, i.e. basic components and rare earth oxide and mistake in table 1 Cross the composition of metal-oxide, weigh various oxide raw material and/or compound corresponding to oxide, fully Mixing, makes compound;Wherein, boron oxide, calcium oxide, strontium oxide and Barium monoxide select the change of its correspondence Compound, the weight portion of corresponding compound is the corresponding parts by weight being converted into according to its oxide content;
Step 102: the compound obtained in step 101 is melted 3 hours at 1200 DEG C, is mixed The melt liquid of material;
Step 103: cooled down on iron plate by the melt liquid of the compound obtained in step 102, after cooling down Glass fragment pulverize, grind, cross 200 mesh sieves, it is thus achieved that host glass powder;
Host glass powder composition is following (gram):
PbO 30.0, B2O330.0, ZnO 20.0, P2O55.0, SiO2 5.0,Al2O35.0, MgO 0.5, CaO 0.5, SrO2.0, BaO 2.0.
The most also include rare earth oxide and the transition gold that seal glass can be made to produce spectral selection absorption characteristic Belonging to oxide, its composition is following (gram):
CeO20.3, Fe2O30.3, Cr2O30.3, Ni2O3 0.3,Co2O30.4, CuO 4.0, FeO 4.0, V2O50.2, MnO 0.2。
Wherein, the gross weight of the gross weight of basic components and described rare earth oxide and transition metal oxide it Between weight ratio be: 100:10.0.
Step 104: preparation fire resistant infilling;
The preparation process of fused silica powder filler is: use three classes or four quartz-like glass through pulverizing, grinding, Cross more than 300 mesh sieves, can be prepared by low-expansion coefficient fused silica powder filler.
Step 105: the fire resistant infilling obtained in the host glass powder obtained in step 103 and step 104 is filled Divide mix homogeneously;
Host glass powder and fused silica powder are 100:5 according to volume ratio, carry out being sufficiently mixed uniformly, make The barium crown sealed glass powder of the present embodiment.
The leaded sealing glass powder of the present embodiment be the coefficient of expansion be 86.8 × 10-7/ DEG C, melting temperature sealing is 520 DEG C Leaded sealing by fusing glass powder.This leaded sealing glass powder has relatively low thermal coefficient of expansion and moderate sealing by fusing Temperature, and there is suction infrared spectral characteristic, can be used for heated light sources is infrared laser or infrared lamp (ripple Long 810~5000 nanometers) light radiation heating process for sealing.
Embodiment 2
A kind of manufacture method of the leaded sealing glass powder with spectral selection absorption characteristic:
Step 101: according to the component of embodiment 2 correspondence, i.e. basic components and rare earth oxide and mistake in table 1 Cross the composition of metal-oxide, weigh various oxide raw material and/or compound corresponding to oxide, fully Mixing, makes compound;Make compound;Wherein, boron oxide, potassium oxide, sodium oxide, lithium oxide and Silver oxide selects the compound of its correspondence, and the weight portion of corresponding compound is for convert according to its oxide content The corresponding parts by weight become;
Step 102: the compound obtained in step 101 is melted 0.5 hour at 800 DEG C, is mixed The melt liquid of material;
Step 103: the melt liquid of compound step 102 obtained cools down on iron plate, after cooling Glass fragment pulverizes, grinds, and crosses 300 mesh sieves, it is thus achieved that host glass powder;
The composition of the host glass powder processed is following (gram):
PbO 87.0, B2O35.0, Bi2O31.0, P2O5 1.0,SiO2 0.5,Al2O3 0.5,K2O 0.5,Na2O 0.5, Li2O 0.5,SnO 0.5,SnO2 0.5,TeO2 0.5,V2O5 0.5Sb2O3 0.5,Ag2 O,PbF2 0.5。
The most also include rare earth oxide and the transition gold that seal glass can be made to produce spectral selection absorption characteristic Belonging to oxide, its composition is following (gram):
CeO22.0, Fe2O32.0, Cr2O3 2.0,Ni2O3 0.2,Co2O30.1, CuO 0.1, FeO 0.5, V2O50.1, MnO 0.1。
Wherein, the gross weight of the gross weight of basic components and described rare earth oxide and transition metal oxide it Between weight ratio be: 100:7.1.
Step 104: preparation fire resistant infilling;
Fire resistant infilling was the calcium metatitanic acid Hydrocerussitum (Ceruse) of 300 mesh sieves
Step 105: by calcium metatitanic acid obtained with step 104 for the host glass powder obtained by step 103 Lead stuffing carries out being sufficiently mixed uniformly;
Host glass powder and calcium metatitanic acid Hydrocerussitum (Ceruse) are that 100:10 carries out being sufficiently mixed uniformly according to volume ratio, make 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/ DEG C, melting temperature sealing is 430 DEG C, There is relatively low melting temperature sealing and good fluidity, ultraviolet light is had selective spectral absorption characteristic, available In the light radiation heating process for sealing that heated light sources is ultraviolet laser or uviol lamp (wavelength 355 nanometer).
Embodiment 3
A kind of manufacture method of the leaded sealing glass powder with spectral selection absorption characteristic:
Step 101: according to the component of embodiment 3 correspondence, i.e. basic components and rare earth oxide and mistake in table 1 Cross the composition of metal-oxide, weigh various oxide raw material and/or compound corresponding to oxide, fully Mixing, makes compound;Wherein, boron oxide, calcium oxide, strontium oxide, Barium monoxide and silver oxide select it Corresponding compound, the weight portion of corresponding compound is the corresponding weight being converted into according to its oxide content Amount number;
Step 102: the compound obtained in step 101 is melted 2 hours at 1100 DEG C, is mixed The melt liquid of material;
Step 103: the melt liquid of compound step 102 obtained cools down on iron plate, after cooling Glass fragment pulverizes, grinds, and crosses 300 mesh sieves, it is thus achieved that host glass powder;
The composition of the host glass powder processed is following (gram):
PbO 46.0, B2O36.0, ZnO 1.3, Bi2O310.0, SiO20.2, Al2O30.2, K2O 0.2, Na2O 0.1, Li2O 0.2, MgO 0.2, CaO 0.2, SrO 0.2, BaO 0.2, SnO 6.0, SnO22.0, TeO23.0, V2O52.0, Sb2O32.0, Ag2O 10.0, PbF2 10.0。
Step 104: choose rare earth oxide and the transition that sealing glass powder can be made to produce characteristic spectrum absorption characteristic In metal-oxide, i.e. table 1, the transition metal oxide of embodiment 3, is adequately mixed and makes mixture;
Mixture composition is following (gram):
Fe2O30.02, Cr2O3 0.02,Ni2O3 0.02,Co2O30.02, CuO 0.02, FeO 0.02.
Step 105: choose fire resistant infilling;
Fire resistant infilling was the beta-eucryptite of 300 mesh sieves;
Step 106: by the mixture obtained in the host glass powder obtained by step 103, step 104 and Beta-eucryptite powder obtained by step 105 carries out being sufficiently mixed uniformly;
Wherein, the proportionate relationship of various powder body is as follows:
Host glass powder obtained by step 103: the percentage by weight of the mixture obtained in step 104 =100:0.12;
The mixture cumulative volume sum obtained in host glass powder obtained in step 103 and step 104: Volume ratio=the 100:15 of the fire resistant infilling obtained in step 105.
Carried out being sufficiently mixed the leaded sealing glass powder making the present embodiment.
The leaded sealing glass powder coefficient of expansion of the present embodiment is 81.2 × 10-7/ DEG C, melting temperature sealing is 460 DEG C, There is relatively low melting temperature sealing and good fluidity, visible ray is had selective spectral absorption characteristic, available In the light radiation heating process for sealing that heated light sources is visible laser (wavelength 380~780 nanometer).
Embodiment 4
A kind of manufacture method of the leaded sealing glass powder with spectral selection absorption characteristic:
Step 101: according to the component of embodiment 4 correspondence, the i.e. composition of basic components in table 1, weigh various Oxide raw material and/or compound corresponding to oxide, be sufficiently mixed, make compound;Wherein, oxidation Boron and silver oxide select the compound of its correspondence, and the weight portion of corresponding compound is according to its oxide content The corresponding parts by weight being converted into;
Step 102: the compound obtained in step 101 is melted 1 hour at 1000 DEG C, is mixed The melt liquid of material;
Step 103: the melt liquid of compound step 102 obtained cools down on iron plate, after cooling Glass fragment pulverizes, grinds, and crosses 300 mesh sieves, it is thus achieved that host glass powder;
The composition of the host glass powder processed is following (%):
PbO 62.9, B2O39.1, ZnO 1.0, Bi2O35.0, P2O53.1, SiO2 1.4,Al2O3 2.4,TeO2 2.0, V2O5 1.0,Sb2O3 1.0,Ag2O 5.5,PbF2 5.5。
Step 104: choose rare earth oxide and the transition that sealing glass powder can be made to produce characteristic spectrum absorption characteristic In metal-oxide, i.e. table 1 in the second component rare earth oxide and transition metal oxide, through filling Divide and be mixed and made into mixture;
Mixture has a following composition:
CeO20.1, Fe2O30.2, Cr2O3 0.2,Ni2O3 2.0,Co2O32.0, CuO 1.0, FeO 1.0, V2O51.0, MnO 1.0。
Step 105: choose fire resistant infilling;
Fire resistant infilling was the cordierite powder of 300 mesh sieves;
Step 106: by the mixture obtained in glass dust obtained in step 103, step 104 and step Cordierite powder obtained by 105 carries out being sufficiently mixed uniformly;
Wherein, the proportionate relationship of various powder body is as follows:
The percentage by weight of the mixture obtained in host glass powder obtained in step 103 and step 104 For: 100:8.5;The mixture that obtains with step 104 of host glass powder obtained by step 103 total The volume ratio of the fire resistant infilling obtained in volume sum and step 105 is: 100:25.
Carried out being sufficiently mixed the leaded sealing glass powder making the present embodiment.
The leaded sealing glass powder coefficient of expansion of the present embodiment is 79.1 × 10-7/ DEG C, melting temperature sealing is 500 DEG C, There is relatively low melting temperature sealing and good fluidity, infrared light is had selective spectral absorption characteristic, available Heat-sealing is added in the light radiation that heated light sources is infrared laser or infrared lamp (wavelength 810~5000 nanometer) Connect technique.
Step 104: choose fire resistant infilling;
Fire resistant infilling was the cordierite powder of 300 mesh sieves;
The composition of 1 three kinds of embodiment seal glasses of table and performance
Table 1 summarize embodiment one, embodiment two, embodiment three and embodiment four totally four kinds of different components and The low temperature with different spectral selection absorption characteristic, the coefficient of expansion, melting temperature sealing and specific insulation is leaded Sealing glass powder.
The beneficial effects of the present invention is: the present invention can be realized glass dust light by the component adjusting glass The adjustment of spectral selectivity absorption characteristic, is adapted to the needs of different light radiation heated light sources;Meanwhile, logical Cross kind and the content adjusting fire resistant infilling, it is achieved the coefficient of expansion, the sealing by fusing work temperature to leaded seal glass The adjustment of degree, thus complete difference by the sealing-in of seal, sealing materials (such as: glass, pottery or metal).
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all the present invention's Within spirit and principle, any modification, equivalent substitution and improvement etc. made, should be included in the present invention's Within protection domain.

Claims (6)

1. a leaded sealing glass powder with spectral selection absorption characteristic, it is characterised in that with leaded Component based on low temperature sealing glass system, added with seal glass can be made to produce spectrum in described basic components The rare earth oxide of selective absorbing characteristic and transition metal oxide;
Described basic components is made up of the leaded low temperature sealing glass of bismuth system;
Between gross weight and described rare earth oxide and the gross weight of transition metal oxide of described basic components Weight ratio be 100:0.12~10.0;
Described rare earth oxide and transition metal oxide are by cerium oxide, iron sesquioxide, chromic oxide, three oxygen Change two nickel, cobalt sesquioxide, copper oxide, ferrous oxide, vanadic anhydride and manganese oxide composition;Each component Weight portion be: CeO20~2.0 part, Fe2O30.02~2.0 part, Cr2O30.02~2.0 part, Ni2O30.02~ 2.0 parts, Co2O30.02~2.0 part, CuO0.02~4.0 parts, FeO 0.02~4.0 parts, V2O50~1.0 part, MnO 0~1.0 parts.
The leaded sealing glass powder with spectral selection absorption characteristic the most according to claim 1, its Being characterised by, the leaded low temperature sealing glass of described bismuth system includes the component of following weight portion: PbO 30.0~87.0 Part, B2O35.0~30.0 parts, ZnO 0~20.0 parts, Bi2O30~10.0 part, P2O50~5.0 part, SiO20.2~5.0 Part, Al2O30.2~5.0 part, K2O 0~0.5 part, Na2O 0~0.5 part, Li2O 0~0.5 part, MgO 0~0.5 Part, CaO 0~0.5 part, SrO 0~2.0 parts, BaO 0~2.0 parts, SnO 0~6.0 parts, SnO20~2.0 Part, TeO20~3.0 part, V2O50~2.0 part, Sb2O30~2.0 part, Ag2O 0~10.0 parts, PbF20~10.0 Part.
3. utilize the leaded sealing glass powder with spectral selection absorption characteristic described in claim 1 to prepare The method of glass dust, it is characterised in that comprise the following steps:
Step 101: according to described basic components and described rare earth oxide and the composition of transition metal oxide, Weigh various oxide raw material and/or compound corresponding to oxide, be sufficiently mixed, make compound;Institute The weight portion stating compound corresponding to oxide is the corresponding weight portion being converted into according to its oxide content Number;
Step 102: the compound obtained 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 obtained in step 102 is carried out solidification cooling, grinds to form base Matter glass dust;
Step 104: choose or prepare the coefficient of expansion for (-100~96) × 10-7/ DEG C fire resistant infilling;
Step 105: the fire resistant infilling that host glass powder step 103 obtained and step 104 obtain is the most mixed Close uniformly.
Preparation method the most according to claim 3, it is characterised in that described host glass powder is with described The volume ratio of fire resistant infilling is: 100:5-25.
5. utilize the leaded sealing glass powder with spectral selection absorption characteristic described in claim 1 to prepare The method of glass dust, it is characterised in that comprise the following steps:
Step 101: according to the composition of described basic components, weigh the various oxides in described basic components and / or compound corresponding to oxide, it is sufficiently mixed, makes compound;The compound that described oxide is corresponding Weight portion be the corresponding parts by weight being converted into according to its oxide content;
Step 102: the compound obtained 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 compound step 102 obtained carries out solidification cooling, grinds to form substrate Glass dust;
Step 104: choose rare earth oxide and the transition that sealing glass powder can be made to produce characteristic spectrum absorption characteristic Metal-oxide, is adequately mixed and makes mixture;
Step 105: choose or prepare the coefficient of expansion for (-100~96) × 10-7/ DEG C fire resistant infilling;
Step 106: by the mixture obtained in the host glass powder obtained by step 103, step 104 and Step 105 gained fire resistant infilling carries out being sufficiently mixed uniformly.
Preparation method the most according to claim 5, it is characterised in that described host glass powder and step The cumulative volume sum of the mixture obtained in 104 with the volume ratio of described fire resistant infilling is: 100:5~25.
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CN117361885B (en) * 2023-10-13 2024-08-16 中建材玻璃新材料研究院集团有限公司 Sealing glass powder for power lithium battery and preparation method thereof

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

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