CN102190445A - Low-temperature acid-resistant sintered glass powder - Google Patents
Low-temperature acid-resistant sintered glass powder Download PDFInfo
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- CN102190445A CN102190445A CN2010101253428A CN201010125342A CN102190445A CN 102190445 A CN102190445 A CN 102190445A CN 2010101253428 A CN2010101253428 A CN 2010101253428A CN 201010125342 A CN201010125342 A CN 201010125342A CN 102190445 A CN102190445 A CN 102190445A
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Abstract
The invention relates to a low-temperature acid-resistant sintered glass powder, which comprises the following raw materials in percentage by weight: 30-70% of SiO2, 1-20% of B2O3, 1-10% of Al2O3, 1-20% of BaO, 1-20% of ZnO, 1-10% of TiO2, 1-20% of Na2O, 1-20% of K2O, 1-10% of CuO, 1-10% of MnO2 and 1-10% of P2O5, wherein the ratio of BaO to ZnO in percentage by weight is more than 1 and less than 2 and the total percentage by weight of Na2O and K2O is 6-25%. The preparation process of the sintered glass powder comprises the following steps: weighing, mixing materials, melting, tabletting, ball-milling and screening. The sintered glass powder has the advantages of low sintering temperature, high airtightness, high chemical durability and high acid resistance, and can be used for the inorganic adhesive phase of electroconductive electronic slurry, the glass paste used for a protective coating and etc.
Description
[technical field]
The invention belongs to chemical technology field, the acidproof sintered glass powder of particularly a kind of low temperature.
[background technology]
Existing electric slurry is with containing a large amount of heavy metal leads in the low-melting-point glass, lead is one of human 6 kinds of metals that use the earliest, it is bigger to human health risk, can gather in vivo and cause lead poisoning, saturnine effect is quite slow and toxicity is hidden, is not easy to be perceiveed before toxicity presents.Lead is a kind of cumulative toxicant, and it is easy to by gastrointestinal absorption, and wherein a part is destroyed blood and made the red blood corpuscle decomposition, and part is diffused into whole body organ and tissue by blood, goes forward side by side into bone.And the lead compound that is deposited in internal organs and the marrow is extremely slow by the speed of discharging in the body, forms chronic poisoning gradually.
In the past, it is the low melting glass that glass etc. contains plumbous oxide that the glass of using as electrocondution slurry mainly is extensive use of lead borosilicate, the glass that contains plumbous oxide because softening temperature is low, mobile, good with the wettability of resistance and electrode, therefore good with connectivity, the stopping property of substrate.
Along with the enhancing of various countries' environmental consciousness, a lot of countries begin to pay close attention to a series of Lead contamination problems that leaded seal glass causes, and have launched respectively relevant policies or have taked related measure.For example American National electronics manufacturing association has finished the exploitation of unleaded preparation electron device, and each main Electronic Products Corporation of Japan has provided the timetable of using lead-free.European Union's electrical equipment and electronics offal treatment method (Waste Electricaland Electronic Equipment.WEEE) propose, and will ban use of the material of heavy metals such as containing Pb, Cd, Hg in 2008.National governments actively support to be engaged in environmental protection important function for of research and development, mainly are that waste reclaims, environmental protection equipment is tax-free, increase the development capital input of heavy metal free environmental protection electronic material.
United States Patent (USP) has been announced a kind of phosphate seal glass P5153151 number, and its mole consists of Li
2O:0～15%, Na
2O:0～20%, K
2O:0～10%, ZnO:0～45%, Ag
2O:0～25%, Tl
2O:0～25%, PbO:0～20%, CuO:0～5%, CaO:0～20%, SrO:0～20%, P
2O
5: 24～36%, Al
2O
3: 0～5%, CeO
2: 0～2%, BaO:0～20%, SnO:0～5%, Sb
2O
3: 0～61%, Bi
2O
3: 0～10%, B
2O
3: 0～10%, the transition temperature of this glass is 300～340 ℃, thermal expansivity is 135～180 * 10
-7/ ℃, the shortcoming of this glass is Tl
2The toxicity of O is very big, and simultaneously, the thermal expansivity of glass is bigger, can not be used for, low-expansion sealing-in.
The spy of Hitachi opens flat 2-267137 and has announced a kind of vanadium oxide (V
2O
5) be seal glass, sealing temperature is less than 400 ℃, thermal expansivity 90 * 10
-7/ ℃ below, but in this glass, plumbous oxide is necessary component, can not satisfy unleaded requirement, simultaneously, also contains the oxide compound of hypertoxic thallium.
U.S. Pat P:20020019303 has proposed a kind of P
2O
5The sealing glass powder of-SnO-ZnO system, the sealing temperature of this glass is 430～500 ℃, because this sealing glass powder need be produced and sealing-in under reducing atmosphere, be unfavorable for commercial application, simultaneously owing to contain the more expensive SnO of a large amount of costs, thereby the application of this seal glass has significant limitation.
The molecular fraction that H7-69672 number disclosed glass of Japanese Patent is formed is: P
2O
5: 25～50%, SnO:30～70%, ZnO:0～25%, add B on this basis
2O
3, WO
3, Li
2O etc., the transition temperature of this glass is 350～450 ℃, thermal expansivity is greater than 120 * 10
-7/ ℃, adopt the method for weighting agent to reduce the coefficient of expansion of glass in the patent, but flowability and resistance to air loss when having influence on glass sealing.
United States Patent (USP) has been announced a kind of lead-free phosphate sealed glass No. 5021366, and its mole consists of: P
2O
5: 30～36%, ZrO
2: 0～45%, alkalimetal oxide 15～25%, alkaline earth metal oxide 15～25% also adds components such as aluminum oxide, stannic oxide and a spot of plumbous oxide.The softening temperature of this glass is 400～430 ℃, and thermal expansivity is 145～170 * 10
-7/ ℃, though the softening temperature of this glass is fit to the eutectic sealing-in, the thermal expansivity of this glass is bigger, can not be used for, low-expansion sealing-in, contains a spot of lead simultaneously, requirement that can not adapted to leadlessization is because precious metal ZrO
2Content higher, therefore aspect cost, do not have advantage equally.
[summary of the invention]
Main purpose of the present invention is to overcome existing electrocondution slurry with the acid proof deficiency of glass powder, provides a kind of low temperature acidproof sintered glass powder, has that sintering temperature is low, resistance to air loss and good characteristics of chemical durability, particularly has good acid resistance.
The objective of the invention is to be achieved through the following technical solutions:
The acidproof sintered glass powder of a kind of low temperature, raw materials by weight consists of: SiO
2Be 30～70%, B
2O
3Be 1～20%, Al
2O
3Be 1～10%, BaO is 1～20%, and ZnO is 1～20%, TiO
2Be 1～10%, Na
2O is 1～20%, K
2O is 1～20%, and CuO is 1～10%, MnO
2Be 1～10%, P
2O
5Be 1～10%;
Described SiO
2Be preferably 35～60%, the best is 50%;
Described B
2O
3Be preferably 5～16%, the best is 10%;
Described Al
2O
3Be preferably 1～5%, the best is 3%;
Described BaO is preferably 5～15%, and the best is 10%;
Described ZnO is preferably 4～14%, and the best is 7%;
Described TiO
2Be preferably 1～5%, the best is 2%;
Described Na
2O is preferably 5～15%, and the best is 8%;
Described K
2O is preferably 2～10%, and the best is 4%;
Described CuO is preferably 1～5%, and the best is 1%;
Described MnO
2Be preferably 1～5%, the best is 1%;
Described P
2O
5Be preferably 1～7%, the best is 4%;
Total weight percent of described BaO/ZnO is less than 2, greater than 1;
Described Na
2O, K
2Total weight percent of O is 6～25%.
Another object of the present invention is to provide a kind of preparation method who is used to produce the acidproof sintered glass powder of above-mentioned a kind of low temperature.
The preparation method of the acidproof sintered glass powder of a kind of low temperature, concrete steps are:
(1) weight percent according to each component takes by weighing each raw material;
(2) with the raw material thorough mixing that is taken by weighing;
(3) mixed compound is put into crucible, put into furnace temperature then and be 1350 ℃～1450 ℃ electric furnace, insulation 4～10h stirs once every 1h at holding stage, stirs 3min at every turn;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours quenching in the cold water into;
(5) sheet or granular glass are put into the ball mill ball milling;
(6) glass powder behind the ball milling is sieved, detects, packs.
The positively effect of the acidproof sintered glass powder of a kind of low temperature of the present invention is:
(1) the present invention is not leaded, satisfies the environmental requirement of WEEE, RoHS instruction, can be used for the bonding phase of electrocondution slurry under the lower glass transition temperature of maintenance;
(2) applied widely, have the performance setting range of broad, simultaneously can also with the glass that conforms to the coefficient of expansion in this temperature, pottery, metal sealing, sealing property is good;
(3) test result shows, not only has thermal expansivity suitable and that be easy to adjust, suitable softening temperature, also has excellent chemical stability, have very strong competitive power aspect unleaded and the excellent performance especially, having the high advantage of cost performance, having market development prospect widely;
(4) acid resistance is good; the inorganic bond phase, supercoat that can be used for the conduction electrons slurry is with glass cream etc.; weather resistance with good air-tightness and chemistry; particularly acid resistance is good; when carrying out the plating processing with acid electroplating liquid; can not cause the resistance variation owing to the dissolving of glass or the infiltration of plating bath; precoated layer glass or secondary coating glass as thick-film resistor are very useful, also can be as the electrode of various electronic components or display element etc. and the supercoat of conductor circuit.
[embodiment]
Below by specific embodiment technical scheme of the present invention is described in detail.
The acidproof sintered glass powder of a kind of low temperature of the present invention, raw materials by weight consists of: SiO
2Be 30～70%, B
2O
3Be 1～20%, Al
2O
3Be 1～10%, BaO is 1～20%, and ZnO is 1～20%, TiO
2Be 1～10%, Na
2O is 1～20%, K
2O is 1～20%, and CuO is 1～10%, MnO
2Be 1～10%, P
2O
5Be 1～10%;
SiO
2Be the netted organizer of glass of the present invention, in order to obtain stability and the good vitreous state of acid resistance, its weight percent contains 30% at least.But, when surpassing 70%,, therefore can not well use because glass is difficult to flow when burning till at low temperatures, be preferably in 35～60% the scope and mix.
Work as B
2O
3When content is very few, B
2O
3Not obvious to the effect that reduces glass softening point, simultaneously, quicken the clarification of glass and the crystallizing power of reduction glass and descend; Work as B
2O
3Greater than 20% o'clock, in the process of fusion cast glass, B
2O
3With the volatilization of water vapour, on the glass metal surface because of B
2O
3Volatilization reduces, and can produce crystallization material skin, works as B
2O
3Introducing is measured when too high, because boron oxygen triangle body increases, the coefficient of expansion of glass etc. increase on the contrary, the acid resistance reduction, and its best scope is 5～16%.
When BaO＜5%, it is not obvious that it can increase the effect of specific refractory power, gloss and chemical stability of glass; When BaO＞15%, can make the clarification difficulty of glass, simultaneously, increased the coefficient of expansion of glass; The existence of an amount of BaO can be quickened the fusing of glass, increases the resistivity and the specific inductivity of glass, and its best scope is 5%～15%.
Work as Al
2O
3＜1 o'clock, it reduced glass crystallization tendency, improved the DeGrain of chemical stability, thermostability, physical strength, hardness and the specific refractory power of glass; Work as Al
2O
3＞5 o'clock, increased the softening temperature of glass, its best scope is 1%～4%.
Work as Na
2O＜5 o'clock are to the fluxing action of glass with to reduce the effect of softening temperature of glass not remarkable; Work as Na
2O＞15 o'clock, the coefficient of expansion increases, and has reduced the chemical stability and the electrical property of glass simultaneously, and its best scope is 5～15%.
The acid resistance of the acidproof sintered glass powder of a kind of low temperature of the present invention is good; the inorganic bond phase, supercoat that can be used for the conduction electrons slurry is with glass cream etc.; weather resistance with good air-tightness and chemistry; particularly acid resistance is good; when carrying out the plating processing with acid electroplating liquid; can not cause the resistance variation owing to the dissolving of glass or the infiltration of plating bath; precoated layer glass or secondary coating glass as thick-film resistor are very useful, also can be as the electrode of various electronic components or display element etc. and the supercoat of conductor circuit.
Embodiment 1
One, the raw material composition is by weight percentage:
SiO
2Be 50%, B
2O
3Be 10%, Al
2O
3Be 3%, BaO is 10%, and ZnO is 7%, TiO
2Be 2%, Na
2O is 8%, K
2O is 4%, and CuO is 1%, MnO
2Be 1%, P
2O
5Be 4%.
Two, preparation method:
(1) weight percent according to each component takes by weighing each raw material;
(2) with the raw material thorough mixing that is taken by weighing;
(3) mixed compound is put into crucible, put into furnace temperature then and be 1380 ℃ electric furnace, insulation 6h stirs once every 1h at holding stage, stirs 3min at every turn;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours quenching in the cold water into;
(5) sheet or granular glass are put into the ball mill ball milling;
(6) glass powder behind the ball milling is sieved, detects, packs.
Three, test result:
BaO/ZnO：1.43
The coefficient of expansion: 85 * 10
-7/ ℃ (300 ℃)
Sintering temperature: 640 ℃
Gloss changes: do not have (before and after the acid attack/2h)
Acid resistance:＜0.3wt% (5wt% sulfuric acid/4h)
Embodiment 2
One, the raw material composition is by weight percentage:
SiO
2Be 34%, B
2O
3Be 11%, Al
2O
3Be 4%, BaO is 15%, and ZnO is 10%, TiO
2Be 5%, Na
2O is 10%, K
2O is 3%, and CuO is 3%, MnO
2Be 3%, P
2O
5Be 2%.
Two, preparation method:
(1) weight percent according to each component takes by weighing each raw material;
(2) with the raw material thorough mixing that is taken by weighing;
(3) mixed compound is put into crucible, put into furnace temperature then and be 1350 ℃ electric furnace, insulation 4h stirs once every 1h at holding stage, stirs 3min at every turn;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours quenching in the cold water into;
(5) sheet or granular glass are put into the ball mill ball milling;
(6) glass powder behind the ball milling is sieved, detects, packs.
Three, test result:
BaO/ZnO：1.5
The coefficient of expansion: 94 * 10
-7/ ℃ (300 ℃)
Sintering temperature: 600 ℃
Gloss changes: do not have (before and after the acid attack/2h)
Acid resistance:＜0.3wt% (5wt% sulfuric acid/4h)
Embodiment 3
One, the raw material composition is by weight percentage:
SiO
2Be 66%, B
2O
3Be 5%, Al
2O
3Be 1%, BaO is 6%, and ZnO is 4%, TiO
2Be 2%, Na
2O is 8%, K
2O is 4%, and CuO is 1%, MnO
2Be 1%, P
2O
5Be 2%.
Two, preparation method:
(1) weight percent according to each component takes by weighing each raw material;
(2) with the raw material thorough mixing that is taken by weighing;
(3) mixed compound is put into crucible, put into furnace temperature then and be 1450 ℃ electric furnace, insulation 8h stirs once every 1h at holding stage, stirs 3min at every turn;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours quenching in the cold water into;
(5) sheet or granular glass are put into the ball mill ball milling;
(6) glass powder behind the ball milling is sieved, detects, packs.
Three, test result:
BaO/ZnO：1.5
The coefficient of expansion: 71 * 10
-7/ ℃ (300 ℃)
Sintering temperature: 680 ℃
Gloss changes: do not have (before and after the acid attack/2h)
Acid resistance:＜0.3wt% (5wt% sulfuric acid/4h)
Embodiment 4
One, the raw material composition is by weight percentage:
SiO
2Be 53%, B
2O
3Be 7%, Al
2O
3Be 2%, BaO is 8%, and ZnO is 6%, TiO
2Be 2%, Na
2O is 12%, K
2O is 6%, and CuO is 1%, MnO
2Be 1%, P
2O
5Be 2%.
Two, preparation method:
(1) weight percent according to each component takes by weighing each raw material;
(2) with the raw material thorough mixing that is taken by weighing;
(3) mixed compound is put into crucible, put into furnace temperature then and be 1350 ℃～1450 ℃ electric furnace, insulation 4～10h stirs once every 1h at holding stage, stirs 3min at every turn;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours quenching in the cold water into;
(5) sheet or granular glass are put into the ball mill ball milling;
(6) glass powder behind the ball milling is sieved, detects, packs.
Three, test result:
BaO/ZnO：1.33
The coefficient of expansion: 97 * 10
-7/ ℃ (300 ℃)
Sintering temperature: 640 ℃
Gloss changes: do not have (before and after the acid attack/2h)
It should be noted last that: above embodiment only is illustrative rather than definitive thereof technical scheme of the present invention, 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 (9)
1. the acidproof sintered glass powder of low temperature is characterized in that raw materials by weight consists of: SiO
2Be 30～70%, B
2O
3Be 1～20%, Al
2O
3Be 1～10%, BaO is 1～20%, and ZnO is 1～20%, TiO
2Be 1～10%, Na
2O is 1～20%, K
2O is 1～20%, and CuO is 1～10%, MnO
2Be 1～10%, P
2O
5Be 1～10%.
2. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 1 is characterized in that described SiO
2Be 35～60%, described B
2O
3Be 5～16%, described Al
2O
3Be 1～5%, described BaO is 5～15%.
3. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 2 is characterized in that described SiO
2Be 50%, described B
2O
3Be 10%, described Al
2O
3Be 3%, described BaO is 10%.
4. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 1 is characterized in that described ZnO is 4～14%, described TiO
2Be 1～5%, described Na
2O is 5～15%, described K
2O elects 2～10% as.
5. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 4 is characterized in that described ZnO is 7%, described TiO
2Be 2%, described Na
2O is 8%, described K
2O elects 4% as.
6. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 1 is characterized in that described CuO is 1～5%, described MnO
2Be 1～5%, described P
2O
5Be 1～7%.
7. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 6 is characterized in that described CuO is 1%, described MnO
2Be 1%, described P
2O
5Be 4%.
8. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 1 is characterized in that total weight percent of described BaO/ZnO is less than 2, greater than 1.
9. the acidproof sintered glass powder of a kind of low temperature as claimed in claim 1 is characterized in that described Na
2O, K
2Total weight percent of O is 6～25%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101253428A CN102190445A (en) | 2010-03-16 | 2010-03-16 | Low-temperature acid-resistant sintered glass powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101253428A CN102190445A (en) | 2010-03-16 | 2010-03-16 | Low-temperature acid-resistant sintered glass powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102190445A true CN102190445A (en) | 2011-09-21 |
Family
ID=44599426
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101253428A Pending CN102190445A (en) | 2010-03-16 | 2010-03-16 | Low-temperature acid-resistant sintered glass powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633435A (en) * | 2012-03-09 | 2012-08-15 | 金招娣 | Lead-free low-temperature glass for manufacturing diode glass shell |
| TWI620204B (en) * | 2015-08-05 | 2018-04-01 | 菲洛公司 | High-k ltcc dielectric compositions and devices and method of forming electronic materials |
| US10100521B2 (en) | 2012-09-11 | 2018-10-16 | 3M Innovative Properties Company | Porous glass roofing granules |
| CN111333329A (en) * | 2018-12-19 | 2020-06-26 | 辽宁省轻工科学研究院有限公司 | Glass powder for sealing armored cable, preparation method thereof and sealing method |
| CN112551904A (en) * | 2020-12-18 | 2021-03-26 | 中国振华集团云科电子有限公司 | Acid-resistant glass powder for end coating of silver paste and preparation method thereof |
| CN114230175A (en) * | 2021-03-25 | 2022-03-25 | 富乔工业股份有限公司 | Glass composition and glass fiber having low coefficient of thermal expansion |
| US11371244B2 (en) | 2012-04-30 | 2022-06-28 | 3M Innovative Properties Company | High solar-reflectivity roofing granules utilizing low absorption components |
-
2010
- 2010-03-16 CN CN2010101253428A patent/CN102190445A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633435A (en) * | 2012-03-09 | 2012-08-15 | 金招娣 | Lead-free low-temperature glass for manufacturing diode glass shell |
| US11371244B2 (en) | 2012-04-30 | 2022-06-28 | 3M Innovative Properties Company | High solar-reflectivity roofing granules utilizing low absorption components |
| US10100521B2 (en) | 2012-09-11 | 2018-10-16 | 3M Innovative Properties Company | Porous glass roofing granules |
| TWI620204B (en) * | 2015-08-05 | 2018-04-01 | 菲洛公司 | High-k ltcc dielectric compositions and devices and method of forming electronic materials |
| CN111333329A (en) * | 2018-12-19 | 2020-06-26 | 辽宁省轻工科学研究院有限公司 | Glass powder for sealing armored cable, preparation method thereof and sealing method |
| CN112551904A (en) * | 2020-12-18 | 2021-03-26 | 中国振华集团云科电子有限公司 | Acid-resistant glass powder for end coating of silver paste and preparation method thereof |
| CN114230175A (en) * | 2021-03-25 | 2022-03-25 | 富乔工业股份有限公司 | Glass composition and glass fiber having low coefficient of thermal expansion |
| CN114230175B (en) * | 2021-03-25 | 2023-09-08 | 富乔工业股份有限公司 | Glass composition with low thermal expansion coefficient and glass fiber |
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Application publication date: 20110921 |