CN103265176B - A kind of sealing glass ceramic, its method for sealing and purposes - Google Patents
A kind of sealing glass ceramic, its method for sealing and purposes Download PDFInfo
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- CN103265176B CN103265176B CN201310187649.4A CN201310187649A CN103265176B CN 103265176 B CN103265176 B CN 103265176B CN 201310187649 A CN201310187649 A CN 201310187649A CN 103265176 B CN103265176 B CN 103265176B
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- sealing
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
Abstract
The present invention relates to a kind of sealing glass ceramic, its raw material comprises SiO
2, ZnO, Al
2o
3, B
2o
3, Na
2cO
3, K
2cO
3, ZrO
2, TiO
2, Li
2cO
3and P
2o
5.The method for sealing of described devitrified glass and its purposes in metal casing for electronic components sealing-in are the invention still further relates to.Sealing glass ceramic provided by the invention changes composition and the consumption of common devitrified glass, and have employed new composite nucleating agent, obtain the devitrified glass of sealing property excellence, thermal expansion matching after sealing-in is good, achieve the fine and close sealing without gas leakage, dielectric loss electric breakdown voltage is high, can meet the requirement of higher standard.Method for sealing technique provided by the invention is simple, does not need the coring of postorder, crystallization process can realize automatic Crystallization, ensure that the intensity of glass, have broad application prospects.
Description
Technical field
The present invention relates to microcrystal glass area, be specifically related to a kind of sealing glass ceramic, use the method for sealing of described devitrified glass and its purposes in metal casing for electronic components sealing-in.
Background technology
The electric property of the electronic devices and components such as rly. is very responsive to surrounding environment, once make moist, corrode or leak, the insulation resistance of device, the degeneration of the performance index such as leakage current or voltage breakdown will be caused, impact is normal to be used, for under severe environment as high temperature, high pressure or strong mechanical vibration time, the probability broken down is more so.At present, the sealing of electronic devices and components adopts glass to stitch realization, as domestic DM305, DM308 borosilicate system etc. more.But this kind of glass powder remains (Fe-29Ni-18Co, thermal expansivity is (4.7 ~ 5.2) × 10 with 4j29
-7dEG C
-1) iron-cobalt-nickel kovar alloy matched performance is poor, easily moisture absorption make moist, the defect such as physical strength is low, poor air-tightness, and leakage rate only can reach 1 × 10
-5paxm
3/ s, can not meet high standard rly. 1 × 10
-9paxm
3the standard of/s.
After the fifties Stookey in latter stage has invented devitrified glass, obtain important application in every field.Compared with traditional glass, devitrified glass has that thermal expansivity variation range is large, electrical insulating property is high, physical strength is high and the feature such as compact structure, and in many performances, exceeded traditional borosilicate system, is the seal, sealing materials of metal device the best.It is as the seal, sealing materials of kovar alloy, there are huge potentiality but at present relevant research or technology less.Therefore, the sealing glass ceramic researching and developing a kind of unleaded free of contamination sealing-in better effects if has very great meaning.
Summary of the invention
For overcoming the deficiency of existing devitrified glass aspect of performance, the object of this invention is to provide a kind of sealing glass ceramic.
Another object of the present invention is to provide a kind of method for sealing of described sealing glass ceramic.
Another object of the present invention is to provide a kind of purposes of described sealing glass ceramic.
Sealing glass ceramic provided by the invention comprises following raw material by weight: 40.0 ~ 70.0 parts of SiO
2, 4.0 ~ 20.0 parts of ZnO, 2.0 ~ 15.0 parts of Al
2o
3, 7.5 ~ 25.0 parts of B
2o
3, 1.0 ~ 5.0 parts of Na
2cO
3, 1.0 ~ 5.0 parts of K
2cO
3, 1.0 ~ 5.0 parts of ZrO
2, 0.1 ~ 3.5 part of TiO
2, 0.3 ~ 6.0 part of Li
2cO
3, 1.0 ~ 5.0 parts of P
2o
5.
Preferably, described sealing glass ceramic comprises following raw material by weight: 50.0 ~ 60.0 parts of SiO
2, 5.5 ~ 15.0 parts of ZnO, 3.0 ~ 10.0 parts of Al
2o
3, 11.5 ~ 20.0 parts of B
2o
3, 2.0 ~ 3.3 parts of Na
2cO
3, 2.0 ~ 5.0 parts of K
2cO
3, 1.0 ~ 2.0 parts of ZrO
2, 0.5 ~ 2.5 part of TiO
2, 0.5 ~ 4.5 part of Li
2cO
3, 1.0 ~ 3.0 parts of P
2o
5.
More preferably, in the raw material of described sealing glass ceramic, Na in mass ratio
2cO
3: K
2cO
3=1: 1 ~ 1.5.
More preferably, in the raw material of described sealing glass ceramic, ZrO in mass ratio
2: P
2o
5=1: 1 ~ 1.5.
Present invention also offers the method for sealing of sealing glass ceramic described in any one of technique scheme, comprise the following steps:
(1) each raw material of described sealing glass ceramic is mixed, add organic solvent and grind until described raw material mixes;
(2) step (1) gained material be heated to 1450 ~ 1550 DEG C and be incubated 2 ~ 6 hours, chilling rolling, then grinding to form glass powder;
(3) in step (2) gained glass powder, add tackiness agent and carry out granulation, then make glass green body;
(4) step (3) gained glass green body is carried out de-waxing at 30 ~ 720 DEG C;
(5) glass green body after de-waxing is carried out sealing-in at 750 ~ 970 DEG C.
Preferably, step (1) described organic solvent is dehydrated alcohol.
Preferably, in chilling described in step (2) and the operation of rolling, quench rate is 1000 ~ 1500 DEG C/sec, and adopted roller mill to carry out chilling and rolling, relative to water-cooled or other types of cooling, cross the contact of the heat-eliminating medium of roller mill and liquid glass more comprehensively, cooling evenly, avoid internal stress that glass cools inequality causes and crystal enrichment is separated out.
Preferably, step (3) described binding agent is PVA (polyvinyl alcohol) or PEG (polyoxyethylene glycol), and its consumption is 2 ~ 8% of step (2) gained glass powder by mass.
Preferably, described step (5) is for carry out sealing-in under nitrogen atmosphere.
Performance after sealing glass ceramic sealing-in of the present invention is significantly improved, and leakage rate is lower, according to 1 × 10
-9paxm
3the standard testing percent of pass of/s is about 92% ~ 93%, therefore, present invention also offers the purposes of described sealing glass ceramic in metal casing for electronic components sealing-in.
Preferably, described electronic devices and components are the electronic devices and components of rly..
Sealing glass ceramic provided by the invention changes composition and the consumption of common devitrified glass, and have employed new composite nucleating agent, obtain the devitrified glass of sealing property excellence, thermal expansion matching after sealing-in is good, achieve the fine and close sealing without gas leakage, dielectric loss electric breakdown voltage is high, can meet the requirement of higher standard.Method for sealing technique provided by the invention is simple, does not need the coring of postorder, crystallization process can realize automatic Crystallization, ensure that the intensity of glass, have broad application prospects.
Accompanying drawing explanation
Fig. 1 is the de-waxing system of sealing-in process described in the embodiment of the present invention;
Fig. 2 is the sealing by fusing system of sealing-in process described in the embodiment of the present invention;
In Fig. 1 and 2, abscissa representing time (hour), ordinate zou represent temperature (DEG C).
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.Wherein used reagent is then interpreted as conventional commercial reagent if no special instructions or obtains according to prior art; Wherein used working method is then interpreted as this area routine operation if no special instructions.
The sealing glass ceramic that embodiment of the present invention provides comprises following raw material by weight: 40.0 ~ 70.0 parts of SiO
2, 4.0 ~ 20.0 parts of ZnO, 2.0 ~ 15.0 parts of Al
2o
3, 7.5 ~ 25.0 parts of B
2o
3, 1.0 ~ 5.0 parts of Na
2cO
3, 1.0 ~ 5.0 parts of K
2cO
3, 1.0 ~ 5.0 parts of ZrO
2, 0.1 ~ 3.5 part of TiO
2, 0.3 ~ 6.0 part of Li
2cO
3, 1.0 ~ 5.0 parts of P
2o
5.。
As preferred embodiment, sealing glass ceramic comprises following raw material by weight: 50.0 ~ 60.0 parts of SiO
2, 5.5 ~ 15.0 parts of ZnO, 3.0 ~ 10.0 parts of Al
2o
3, 11.5 ~ 20.0 parts of B
2o
3, 2.0 ~ 3.3 parts of Na
2cO
3, 2.0 ~ 5.0 parts of K
2cO
3, 1.0 ~ 2.0 parts of ZrO
2, 0.5 ~ 2.5 part of TiO
2, 0.5 ~ 4.5 part of Li
2cO
3, 1.0 ~ 3.0 parts of P
2o
5.
Li in sealing glass ceramic raw material described in embodiment of the present invention
2cO
3, Na
2cO
3and K
2cO
3li will be broken down in high melt process
2o, Na
2o and K
2o, can be used as the main ingredient of devitrified glass, and the carbon dioxide simultaneously discharged in decomposition course also contributes to clarification, the deslagging of glass.Na in glass
2o, K
2o can also play the effect reducing glass high temperature viscosity, is conducive to levelling during glass sealing operation, works as Na
2cO
3and K
2cO
3mass ratio be 1: 1 ~ 1.5, the effect for glass sealing operation is best.Li in glass
2o can make the crystallization behavior of glass become gentle and more even, makes the crystal of precipitation finer and smoother, the distribution of crystal fine particle and size also evenly, contribute to intensity and the toughness of reinforcing glass.
P in sealing glass ceramic raw material of the present invention
2o
5,zrO
2for composite nucleating agent, can crystal be made to be more prone to ZnAl in the operation of glass heat-insulating crystallization
2o
4(relative to ZnB
2o
4, ZnAl
2o
4the existence of crystal makes chemical durability of glass better, and strength of glass is higher) precipitation, farthest suppress ZnB
2o
4the generation of crystal and the (ZnB in crystallize out that grows up
2o
4volume ratio be less than 10%).And, P
2o
5and ZrO
2also can be used as the catalyzer of devitrification of glass, making glass crystallization behavior when lowering the temperature in advance, and extend crystallization interval, make crystallization behavior be tending towards relaxing, evenly.In addition, P
2o
5,zrO
2when acting in conjunction is nucleating agent, respective consumption also has very crucial effect, and the two weight ratio is 1: 1 ~ 1.5 time, and the effect as nucleating agent and catalyzer is best.
The method for sealing that embodiment of the present invention provides, comprises the following steps:
(1) each raw material of described sealing glass ceramic is mixed, add organic solvent and grind until described raw material mixes;
(2) step (1) gained material be heated to 1450 ~ 1550 DEG C and be incubated 2 ~ 6 hours, chilling rolling, then grinding to form glass powder;
(3) in step (2) gained glass powder, add tackiness agent and carry out granulation, then make glass green body;
(4) step (3) gained glass green body is carried out de-waxing at 30 ~ 720 DEG C;
(5) glass green body after de-waxing is carried out sealing-in at 750 ~ 970 DEG C.
As preferred embodiment, method for sealing of the present invention comprises the following steps:
(1) each raw material of sealing glass ceramic is mixed, (add-on of ethanol is not particularly limited to add a certain amount of dehydrated alcohol, as long as it contributes to making each raw material dispersed), ball milling is until each feed composition mixes;
(2) step (1) gained material be heated to 1450 ~ 1550 DEG C and be incubated 3 ~ 5 hours, the glass metal obtained is cooled (rate of cooling is about 1000 ~ 1500 DEG C/sec) rapidly by roller mill and is rolled and obtains flap, then by gained flap conveniently required particle diameter grind to form glass powder (being generally 2 ~ 10 microns);
(3) add in the glass powder of step (2) gained mass percent be 2 ~ 8% tackiness agent and routinely granulation process carry out granulation, then make glass green body; Wherein, sealing glass ceramic field any one binding agent existing selected by binding agent, preferably polyethylene alcohol (PVA) binding agent or polyoxyethylene glycol (PEG) binding agent;
(4) step (3) gained glass green body is carried out de-waxing according to the de-waxing system shown in Fig. 1 at 30 ~ 720 DEG C;
(5) glass green body after de-waxing is carried out sealing-in according to the sealing by fusing system shown in Fig. 2 in the atmosphere of nitrogen protection at 750 ~ 970 DEG C.
Embodiment
The composition of raw materials of sealing glass ceramic is as shown in table 1.
Glass ingredient quality proportioning (mass parts) in each embodiment of table 1
| Composition | SiO 2 | ZnO | Al 2O 3 | Li 2CO 3 | B 2O 3 | Na 2CO 3 | K 2CO 3 | ZrO 2 | TiO 2 | P 2O 5 |
| Embodiment 1 | 54.00 | 12.00 | 3.50 | 4.20 | 15.33 | 3.05 | 3.92 | 2.00 | 2.00 | 3.00 |
| Embodiment 2 | 57.50 | 8.66 | 5.72 | 0.90 | 16.25 | 3.05 | 3.92 | 2.00 | 2.00 | 2.85 |
| Embodiment 3 | 54.30 | 10.40 | 8.33 | 2.20 | 15.30 | 2.05 | 2.42 | 1.50 | 2.00 | 2.25 |
| Embodiment 4 | 41.50 | 15.30 | 13.40 | 5.08 | 9.23 | 2.80 | 4.02 | 4.57 | 1.50 | 4.60 |
| Embodiment 5 | 64.20 | 5.60 | 2.41 | 1.10 | 20.08 | 1.06 | 1.10 | 1.50 | 2.53 | 2.12 |
| Embodiment 6 | 45.00 | 11.25 | 3.00 | 0.50 | 8.00 | 2.20 | 2.45 | 1.00 | 0.50 | 1.20 |
| Embodiment 7 | 67.10 | 18.50 | 14.00 | 5.65 | 23.40 | 4.50 | 5.00 | 5.00. | 3.35 | 5.00 |
Embodiment 1
The sealing-in process of embodiment 1 devitrified glass is as follows:
(1) mixed by each raw material of the sealing glass ceramic described in embodiment in table 11, add dehydrated alcohol, ball milling is until each feed composition mixes.
(2) step (1) gained material be heated to about 1500 DEG C and be incubated about 4 hours, the glass metal obtained is cooled (rate of cooling is about 1200 DEG C/sec) rapidly by roller mill and is rolled and obtains flap, then gained flap is ground to form the glass powder that particle diameter is 2-10 micron.
(3) in the glass powder of step (2) gained, add the PVA tackiness agent that mass percent is about 5% carry out granulation, then make glass green body.
(4) step (3) gained glass green body is carried out de-waxing according to the de-waxing system shown in Fig. 1.
(5) glass green body after de-waxing is carried out sealing-in according to the sealing by fusing system shown in Fig. 2 under the atmosphere of nitrogen protection.
Embodiment 2
The sealing-in process of embodiment 2 devitrified glass is as follows:
(1) mixed by each raw material of the sealing glass ceramic described in embodiment in table 12, add dehydrated alcohol, ball milling is until each feed composition mixes.
(2) step (1) gained material be heated to about 1450 DEG C and be incubated about 5 hours, the glass metal obtained is cooled (rate of cooling is about 1150 DEG C/sec) rapidly by roller mill and is rolled and obtains flap, then gained flap is ground to form the glass powder that particle diameter is 2-10 micron.
(3) in the glass powder of step (2) gained, add the PVA tackiness agent that mass percent is about 5% carry out granulation, then make glass green body.
(4) step (3) gained glass green body is carried out de-waxing according to the de-waxing system shown in Fig. 1.
(5) glass green body after de-waxing is carried out sealing-in according to the sealing by fusing system shown in Fig. 2 under the atmosphere of nitrogen protection.
Embodiment 3
The sealing-in process of embodiment 3 devitrified glass is as follows:
(1) mixed by each raw material of the sealing glass ceramic described in embodiment in table 13, add dehydrated alcohol, ball milling is until each feed composition mixes.
(2) step (1) gained material be heated to about 1550 DEG C and be incubated about 3 hours, the glass metal obtained is cooled (rate of cooling is about 1400 DEG C/sec) rapidly by roller mill and is rolled and obtains flap, then gained flap is ground to form the glass powder that particle diameter is 2-10 micron.
(3) in the glass powder of step (2) gained, add the PEG tackiness agent that mass percent is about 5% carry out granulation, then make glass green body.
(4) step (3) gained glass green body is carried out de-waxing according to the de-waxing system shown in Fig. 1.
(5) glass green body after de-waxing is carried out sealing-in according to the sealing by fusing system shown in Fig. 2 under the atmosphere of nitrogen protection.
Embodiment 4
The sealing-in process of embodiment 4 devitrified glass is with embodiment 1.
Embodiment 5
The sealing-in process of embodiment 5 devitrified glass is with embodiment 2.
Embodiment 6
The sealing-in process of embodiment 6 devitrified glass is with embodiment 3.
Embodiment 7
The sealing-in process of embodiment 7 devitrified glass is with embodiment 1.
Experimental example
Test according to standard described in GB 9622.1 ~ 9622.11 and testing method sealing-in effect after sealing-in, result as Table 2,3.
The glass wetting test parameter of each embodiment of table 2
Table 3: the glass properties detect parameters of each embodiment
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (9)
1. a sealing glass ceramic, is characterized in that, comprises following raw material by weight: 50.0 ~ 60.0 parts of SiO
2, 5.5 ~ 15.0 parts of ZnO, 3.0 ~ 10.0 parts of Al
2o
3, 11.5 ~ 20.0 parts of B
2o
3, 2.0 ~ 3.3 parts of Na
2cO
3, 2.0 ~ 5.0 parts of K
2cO
3, 1.0 ~ 2.0 parts of ZrO
2, 0.5 ~ 2.5 part of TiO
2, 0.5 ~ 4.5 part of Li
2cO
3, 1.0 ~ 3.0 parts of P
2o
5.
2. sealing glass ceramic according to claim 1, is characterized in that, in the raw material of described sealing glass ceramic, and Na in mass ratio
2cO
3: K
2cO
3=1: 1 ~ 1.5.
3. sealing glass ceramic according to claim 1, is characterized in that, in the raw material of described sealing glass ceramic, and ZrO in mass ratio
2: P
2o
5=1: 1 ~ 1.5.
4. the method for sealing of sealing glass ceramic described in any one of claim 1-3, is characterized in that, comprise the following steps:
(1) each raw material of described sealing glass ceramic is mixed, add organic solvent and grind until described raw material mixes;
(2) step (1) gained material be heated to 1450 ~ 1550 DEG C and be incubated 2 ~ 6 hours, chilling rolling, then grinding to form glass powder;
(3) in step (2) gained glass powder, add tackiness agent and carry out granulation, then make glass green body;
(4) step (3) gained glass green body is carried out de-waxing at 30 ~ 720 DEG C;
(5) glass green body after de-waxing is carried out sealing-in at 750 ~ 970 DEG C.
5. method for sealing according to claim 4, is characterized in that, step (1) described organic solvent is dehydrated alcohol.
6. method for sealing according to claim 4, is characterized in that, step (3) described tackiness agent is PVA or PEG, and its consumption is 2 ~ 8% of step (2) gained glass powder by mass.
7. method for sealing according to claim 4, is characterized in that, described step (5) for carry out sealing-in under the atmosphere of nitrogen.
8. the purposes of sealing glass ceramic in metal casing for electronic components sealing-in described in any one of claim 1-3.
9. purposes according to claim 8, is characterized in that, described electronic devices and components are the electronic devices and components of rly..
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310187649.4A CN103265176B (en) | 2013-05-20 | 2013-05-20 | A kind of sealing glass ceramic, its method for sealing and purposes |
| PCT/CN2013/088213 WO2014187100A1 (en) | 2013-05-20 | 2013-11-29 | Raw material for sealing microcrystalline glass, and sealing method therefor |
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|---|---|---|---|
| CN201310187649.4A CN103265176B (en) | 2013-05-20 | 2013-05-20 | A kind of sealing glass ceramic, its method for sealing and purposes |
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| CN103265176B true CN103265176B (en) | 2015-10-14 |
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| WO (1) | WO2014187100A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265176B (en) * | 2013-05-20 | 2015-10-14 | 京东方科技集团股份有限公司 | A kind of sealing glass ceramic, its method for sealing and purposes |
| CN104529164A (en) * | 2014-12-17 | 2015-04-22 | 中国科学院上海硅酸盐研究所 | Devitrification type high-expansion sealing glass powder as well as preparation method and application thereof |
| CN106082672A (en) * | 2016-06-15 | 2016-11-09 | 山东智汇专利运营有限公司 | A kind of teaching devitrified glass and preparation method thereof |
| CN106219982B (en) * | 2016-07-26 | 2019-04-23 | 浙江宇清热工科技股份有限公司 | For the glaze and its application method of combination between a kind of devitrified glass |
| CN108164145A (en) * | 2016-12-07 | 2018-06-15 | 辽宁省轻工科学研究院 | A kind of easy crystallization can cut down sealing glass material and its preparation method and application |
| CN108238723A (en) * | 2016-12-26 | 2018-07-03 | 西安宏星电子浆料科技有限责任公司 | Solar energy crystal silicon battery back silver paste lead-free electronic glass powder and preparation method thereof |
| CN114656155B (en) * | 2022-04-29 | 2023-09-08 | 中国科学院上海硅酸盐研究所 | Low-dielectric low-loss low-expansion glass material and preparation method and application thereof |
| CN116535097A (en) * | 2023-04-28 | 2023-08-04 | 武汉理工大学 | Glass powder, conductive copper paste and multilayer ceramic capacitor for MLCC and preparation method |
| CN117410517B (en) * | 2023-12-15 | 2024-03-15 | 中石油深圳新能源研究院有限公司 | Seal for solid oxide fuel cell and method for producing the same |
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- 2013-11-29 WO PCT/CN2013/088213 patent/WO2014187100A1/en active Application Filing
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|---|---|
| CN103265176A (en) | 2013-08-28 |
| WO2014187100A1 (en) | 2014-11-27 |
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