CN100412017C - Lead-free sealing glass and producing method - Google Patents
Lead-free sealing glass and producing method Download PDFInfo
- Publication number
- CN100412017C CN100412017C CNB200310103589XA CN200310103589A CN100412017C CN 100412017 C CN100412017 C CN 100412017C CN B200310103589X A CNB200310103589X A CN B200310103589XA CN 200310103589 A CN200310103589 A CN 200310103589A CN 100412017 C CN100412017 C CN 100412017C
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- Prior art keywords
- oxide
- weight percent
- glass
- vitreum
- sealed glass
- Prior art date
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- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title claims description 12
- 239000005394 sealing glass Substances 0.000 title abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 58
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 229910052788 barium Inorganic materials 0.000 claims description 24
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 11
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 5
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 5
- 230000006641 stabilisation Effects 0.000 claims description 4
- 238000011105 stabilization Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- 230000004927 fusion Effects 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 3
- 229910001392 phosphorus oxide Inorganic materials 0.000 claims 3
- VSAISIQCTGDGPU-UHFFFAOYSA-N tetraphosphorus hexaoxide Chemical compound O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 claims 3
- 239000011575 calcium Substances 0.000 claims 2
- 239000011787 zinc oxide Substances 0.000 claims 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 229910010413 TiO 2 Inorganic materials 0.000 claims 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims 1
- 150000001552 barium Chemical class 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 125000005843 halogen group Chemical group 0.000 claims 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 229910001930 tungsten oxide Inorganic materials 0.000 claims 1
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 abstract description 8
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 4
- 238000007789 sealing Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 3
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 7
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229910052714 tellurium Inorganic materials 0.000 description 3
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 3
- 229910052716 thallium Inorganic materials 0.000 description 3
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005816 glass manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- WKMKTIVRRLOHAJ-UHFFFAOYSA-N oxygen(2-);thallium(1+) Chemical compound [O-2].[Tl+].[Tl+] WKMKTIVRRLOHAJ-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910003438 thallium oxide Inorganic materials 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/16—Silica-free oxide glass compositions containing phosphorus
- C03C3/21—Silica-free oxide glass compositions containing phosphorus containing titanium, zirconium, vanadium, tungsten or molybdenum
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
- C03C3/247—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron containing fluorine and phosphorus
Abstract
The present invention relates to sealing glass without lead. The present invention is a glass body which is formed after vanadium oxide (V2O5), phosphorus oxide (P2O5) and antimony oxide (Sb2O3) are mutually mixed to be melted and cooled. The present invention comprises by weight percentage: 30% to 70% of vanadium oxide (V2O5), 10%to 30% of phosphorus oxide (P2O5), and 0.5% to 25% of antimony oxide (Sb2O3). A preparation method of the present invention at least comprises: weighing the vanadium oxide (V2O5), the phosphorus oxide (P2O5) and the antimony oxide (Sb2O3) by the weight percentage, and then, fully mixing the components so that a mixed material is prepared; melting the mixed material for 2 to 3 hours at the temperature of 800 DEG C to 1200 DEG C; cooling and solidifying melted liquid. The sealing glass without lead, which is supplied by the present invention, can directly seal a vacuum glass product needing sealing (such as VFD, PDP, CRT, etc.) in a nontoxicity and no pollution mode and can adjust component mixture ratio according to different temperature and thermal expansion characteristics of the sealed product so that the sealing requirements for various materials is met.
Description
Technical field
The present invention relates to a kind of barium crown sealed glass, particularly a kind of not leaded and have low melting point, low expansion character, can be used for various vacuum glass devices are carried out the manufacture method of glass and this glass of sealing-in.
Background technology
In the production process of vacuum glass goods, need have usually than low melting point and more low-expansion glass or glass powder as seal, sealing materials.
Before this, a large amount of seal glasses that use all are the low-melting point sealing glass of plumbous zinc system (PbO-ZnO), though this glass can satisfy the sealing-in requirement of vacuum glass device preferably, but because plumbous influence to environment and human health, therefore, for providing lead-free sealing glass material, vacuum glass product manufacturing become the problem that must solve as early as possible.
At present, existing in the world seal glass and glass powder have following several usually.
The spy of Hitachi opens flat 2-267137 and discloses a class vanadium oxide (V
2O
5) be glass.The coefficient of expansion of this glass is 90 * 10
-7/ ℃ below, sealing temperature is below 400 ℃, it mainly acts on is to prepare the coefficient of expansion in (30～45) * 10
-7/ ℃ about sealing glass powder.But in this product, plumbous oxide is the neccessary composition as component, thereby can't satisfy unleaded requirement, simultaneously, owing to also contain the oxide compound of hypertoxic thallium (Tl) in this product, and the price of Tl is comparatively expensive, therefore, this glass and uneconomical again with the i.e. not environmental protection of glass powder of this glass making can only be used for special vacuum glass goods.
In addition, the fair 5-85490 in flat Hitachi proposes a class V
2O
5-Tl
2O-TeO
2-R
2O glass, main component are V
2O
5, P
2O
5, contain the oxide compound of sodium, potassium, rubidium, caesium, tellurium etc. simultaneously, can finish 400～500 ℃ sealing-in, the coefficient of expansion (70～130) * 10
-7/ ℃.Though not leaded in the composition of this glass, owing to contain a certain amount of highly toxic substance thallium oxide (TlO
2) and noble metal tellurium (Te) etc., thereby cost is very high.It mainly is used as the seal, sealing materials and the magnetic gap compaction material of high-performance magnetic head.
Have, the U.S. Pat 2002019303 of NIPPON electronic glass application has proposed a kind of P again
2O
5The sealing glass powder of-SnO-ZnO, 430～500 ℃ of sealing temperatures.But because this glass powder contains a large amount of SnO, and oxidation easily, need under reducing atmosphere conditions such as complete nitrogen, produce and sealing-in, thereby be difficult to carry out industrialization and postorder sealing-in application, simultaneously, SnO is also relatively more expensive.Owing to have above defective, make the use of this glass be subjected to bigger restriction.
In the research of barium crown sealed glass, adopt bismuth oxide (Bi in addition
2O
3) substitute the bismuth glass of plumbous oxide.But, owing to use bismuth oxide, make manufacturing cost increase greatly, and the coefficient of expansion of this glass is too big, be difficult to regulate the requirement that reaches with the sealing-in that is complementary by the coefficient of expansion of sealing-in product in actual applications.
Summary of the invention
Main purpose of the present invention is to provide a kind of barium crown sealed glass at the defective that contains lead or thallium or noble metal and oxide compound thereof in the above-mentioned seal glass, this seal glass does not only contain lead, and do not contain highly toxic substances such as tellurium or thallium, do not contain noble metal and oxide compound thereof simultaneously yet.
Another object of the present invention is to provide a kind of method that is used to make above-mentioned barium crown sealed glass.
The objective of the invention is to be achieved through the following technical solutions:
A kind of barium crown sealed glass, it is by vanadium oxide (V at least
2O
5), phosphorus oxide (P
2O
5) and weisspiessglanz (Sb
2O
3) mix the vitreum of after the fusion cooling, being formed mutually; Described vanadium oxide (V
2O
5) weight percent be 30%-70%; Described phosphorus oxide (P
2O
5) weight percent be 21%-30%; Described weisspiessglanz (Sb
2O
3) weight percent be 0.5%-25%; Also comprise bismuth oxide Bi in the described vitreum
2O
3, its weight percent is 0.5%-4.5%.
In above-mentioned barium crown sealed glass, can also sneak into stabilization component and halogenide according to specific requirement.
The manufacture method of above-mentioned barium crown sealed glass may further comprise the steps at least:
Step 1: take by weighing vanadium oxide (V according to weight percent
2O
5), phosphorus oxide (P
2O
5), bismuth oxide Bi
2O
3And weisspiessglanz (Sb
2O
3) after carry out thorough mixing, make compound;
Step 2: described compound was melted 2-3 hour down at 800 ℃～1200 ℃;
Step 3: the liquid to fusing in the step 2 carries out cooling curing, makes vitreum.
Vitreum can be made tabular, column or directly make powdery according to sealing-in product characteristics and requirement.
Barium crown sealed glass provided by the present invention can directly carry out nontoxic, pollution-free sealing-in to the vacuum glass goods (as VFD, PDP, CRT etc.) that need sealing-in, also can be according to difference by the temperature of sealing-in product, thermal expansion character, adjustment set of dispense ratio satisfies the sealing-in requirement of multiple differing materials.The requirement of for example various glass, pottery, intermetallic and mutual sealing-in.
Description of drawings
Fig. 1 is the manufacturing process flow diagram of barium crown sealed glass involved in the present invention;
Embodiment
Below, the composition by specific embodiment and the description of manufacturing processed and the present invention is described in further detail in conjunction with the accompanying drawings.
Embodiment
Present embodiment composed as follows:
Component title weight percent
Vanadium oxide (V
2O
5) 58%
Phosphorus oxide (P
2O
5) 31.5%
Weisspiessglanz (Sb
2O
3) 10%
After above three kinds of components are mixed mutually, 800 ℃ down fusing carry out the moulding cooling and promptly can be made into barium crown sealed glass after 2 hours.
On the basis of the foregoing description, can be by adding other compositions, adjusting the barium crown sealed glass that component ratio obtains multiple each tool characteristic.Below, exemplify six kinds of barium crown sealed glass, further describe by form.
Form one
| No. one | No. two | No. three | No. four | No. five | No. six | |
| V 2O 5 | 58 | 54 | 60 | 51.5 | 57 | 50 |
| P 2O 5 | 31.5 | 22.5 | 30 | 19.5 | 21 | 30 |
| Sb 2O 3 | 10 | 15 | 6 | 15 | 13 | 9 |
| Bi 2O 3 | -- | 3 | 6 | 3 | 4.5 | |
| Al 2O 3 | -- | 2 | 2 | 5 | 0.5 | 2 |
| SiO2 | -- | 1.5 | 1 | 1 | 0.5 | 2 |
| ZnO | -- | 2 | 1 | 2 | 1.5 | 1 |
| SnCl 2 | -- | -- | -- | -- | 1.5 | 1.5 |
| B 2O 3 | 0.5 | -- | -- | -- | -- | -- |
| WO 3 | -- | -- | -- | -- | 1 | -- |
| F - | -- | -- | -- | -- | 1 | -- |
| Glass α (* 10 -7/℃) | 95 | 72.5 | 103 | 89 | 110 | 105 |
The manufacture method of six kinds of barium crown sealed glass that exemplified in the above table one is identical, and its process is with reference to schema shown in Figure 1.
At first, starting material are taken by weighing each component according to the weight percent described in the form one; Then with the raw material thorough mixing; Mixture was melted 2～3 hours under 800 ℃～1200 ℃ temperature; Glass metal with fusing carries out forming processes at last, makes tabular or column, also the glass metal of fusing can be dried through water is fried, and pulverize, sieves and make powdery, makes it can be used in the occasion that needs glass powder to carry out sealing-in.
In form one, the component of a barium crown sealed glass is on the basis of the foregoing description, has added 0.5% boron oxide B
2O
3As the stabilization component.The component of other five kinds of barium crown sealed glass all is at vanadium oxide (V
2O
5), phosphorus oxide (P
2O
5), weisspiessglanz (Sb
2O
3) on the basis of these three kinds of basal components, by adding other different compositions and adjusting the barium crown sealed glass that proportion relation between each component obtains having the different coefficients of expansion, its coefficient of expansion is in (72.5-110) * 10
-7/ ℃ between.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (5)
1. barium crown sealed glass, it is characterized in that: it is by vanadium oxide V at least
2O
5, phosphorus oxide P
2O
5And weisspiessglanz Sb
2O
3Mix the vitreum of after the fusion cooling, being formed mutually;
Described vanadium oxide V
2O
5Weight percent be 30%-70%; Described phosphorus oxide P
2O
5Weight percent be 21%-30%; Described weisspiessglanz Sb
2O
3Weight percent be 0.5%-25%;
Also comprise bismuth oxide Bi in the described vitreum
2O
3, its weight percent is 0.5%-4.5%.
2. barium crown sealed glass according to claim 1 is characterized in that: comprise also in the described vitreum that weight percent is not higher than 40% stabilization component; Described stabilization component is a kind of oxide compound or is mixed by more than one oxide compound and to form;
The weight percent that described oxide compound is included in the described vitreum is no more than 10% silicon oxide sio
2Or zinc oxide ZnO or aluminium oxide Al
2O
3Or zirconium white ZrO
2Or boron oxide B
2O
3Or titanium oxide TiO
2And the weight percent in described vitreum is no more than 5% Tungsten oxide 99.999 WO
3Or alkalimetal oxide.
3. barium crown sealed glass according to claim 1 and 2, it is characterized in that: the halogenide or its halid arbitrary combination body that also comprise tin Sn or zinc Zn or calcium Ca in this barium crown sealed glass, wherein, the weight percent of each halogenide in described vitreum is no more than 5%.
4. barium crown sealed glass according to claim 1 is characterized in that: described vitreum is tabular or column or powdery.
5. the manufacture method of a barium crown sealed glass, it is characterized in that: described manufacture method is the method that is used to make the arbitrary described barium crown sealed glass of aforesaid right requirement 1-4, and this manufacture method may further comprise the steps at least:
Step 1: take by weighing vanadium oxide V according to weight percent
2O
5, phosphorus oxide P
2O
5, bismuth oxide Bi
2O
3And weisspiessglanz Sb
2O
3After carry out thorough mixing, make compound;
Step 2: described compound was melted 2-3 hour down at 800 ℃～1200 ℃;
Step 3: the liquid to fusing in the step 2 carries out cooling curing, makes vitreum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310103589XA CN100412017C (en) | 2003-11-11 | 2003-11-11 | Lead-free sealing glass and producing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310103589XA CN100412017C (en) | 2003-11-11 | 2003-11-11 | Lead-free sealing glass and producing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1616365A CN1616365A (en) | 2005-05-18 |
| CN100412017C true CN100412017C (en) | 2008-08-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200310103589XA Expired - Lifetime CN100412017C (en) | 2003-11-11 | 2003-11-11 | Lead-free sealing glass and producing method |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265023B (en) * | 2007-03-15 | 2010-05-26 | 北京印刷学院 | Vanadium-silver low melting glass and conductive slurry containing the glass |
| CN102173593B (en) * | 2011-02-12 | 2013-03-27 | 刘国正 | Lead-free glass powder, preparation method and application thereof |
| CN107140839A (en) * | 2017-06-05 | 2017-09-08 | 西安工程大学 | A kind of lead-free glass powder with low melting point and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6136135A (en) * | 1984-07-27 | 1986-02-20 | Hitachi Ltd | Filling glass for magnetic recording head |
| JPS6228128A (en) * | 1985-07-31 | 1987-02-06 | Shimano & Co Ltd | Manufacture of oval gear |
| JPS6272543A (en) * | 1985-09-27 | 1987-04-03 | Hitachi Ltd | Glass composition |
| JPH02149446A (en) * | 1988-11-29 | 1990-06-08 | Matsushita Electric Ind Co Ltd | Sealing composition and crystal resonator |
| JPH02267137A (en) * | 1989-04-06 | 1990-10-31 | Hitachi Ltd | Sealing material |
-
2003
- 2003-11-11 CN CNB200310103589XA patent/CN100412017C/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6136135A (en) * | 1984-07-27 | 1986-02-20 | Hitachi Ltd | Filling glass for magnetic recording head |
| JPS6228128A (en) * | 1985-07-31 | 1987-02-06 | Shimano & Co Ltd | Manufacture of oval gear |
| JPS6272543A (en) * | 1985-09-27 | 1987-04-03 | Hitachi Ltd | Glass composition |
| JPH02149446A (en) * | 1988-11-29 | 1990-06-08 | Matsushita Electric Ind Co Ltd | Sealing composition and crystal resonator |
| JPH02267137A (en) * | 1989-04-06 | 1990-10-31 | Hitachi Ltd | Sealing material |
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| CN1616365A (en) | 2005-05-18 |
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