CN101717197A - Lead-free glass powder and preparation method thereof and application thereof in computer field - Google Patents

Lead-free glass powder and preparation method thereof and application thereof in computer field Download PDF

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Publication number
CN101717197A
CN101717197A CN200910198372A CN200910198372A CN101717197A CN 101717197 A CN101717197 A CN 101717197A CN 200910198372 A CN200910198372 A CN 200910198372A CN 200910198372 A CN200910198372 A CN 200910198372A CN 101717197 A CN101717197 A CN 101717197A
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glass powder
lead
free glass
bao
zno
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CN200910198372A
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Inventor
刘荣辉
邵国金
张玉花
薛冰
陈红军
李胜春
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郑庆云
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Abstract

The invention discloses lead-free glass powder and a preparation method and application thereof in the computer field. The glass powder comprises the following materials by weight percentage: 30-50% of SiO2, 1-10% of B2O3, 1-10% of Al2O3, 1-20% of BaO, 1-10% of ZnO, 1-10% of TiO2, 1-20% of Na2O, 1-10% of Li2O, 1-5% of ZrO2, 1-10% of V2O5 and 0.1-2% of Co3O4. The preparation process comprises the steps of weighing, mixing materials, melting, tabletting, ball-milling and sieving. The invention has the advantages of low sintering temperature, favorable air-tightness and chemical durability and particularly excellent acid resistance, can be used for the inorganic binder phase of a conductive electronic slurry, the glass paste for a protective coat, and the like, and has excellent air-tightness and chemical durability.

Description

A kind of lead-free glass powder and preparation method thereof and application in computer realm
[technical field]
The invention belongs to chemical technology field, particularly a kind of lead-free glass powder and preparation method thereof and application in computer realm.
[background technology]
Electric slurry is a base mateiral of making thick film element, is a kind of paste that is mixed through three-roll rolling by pressed powder and organic solvent.By the purposes difference, be divided into dielectric paste, resistance slurry and conductor paste: be divided into ceramic substrate, polymer matrix film, glass substrate and metal-insulator substrate electric slurry etc. by the substrate kind; By the sintering temperature difference, can be divided into high temperature, middle gentle oven drying at low temperature electric slurry; By the purposes difference, can be divided into universal electric slurry (making general thick film circuit) and special electronic slurry (stainless steel substrate electric slurry, thermistor slurry); Price by conductive phase is divided into precious metal electric slurry (silver-colored palladium, ruthenium system and gold paste etc.) and base metal electric slurry (molybdenum manganese slurry).
Electrocondution slurry is a base mateiral of making thick film element, is a kind of paste (but association becomes appearance such as toothpaste, paint) that is mixed through three-roll rolling by pressed powder and organic solvent.The electrocondution slurry product integrates metallurgy, chemical industry, electronic technology, it is a kind of electronic functional material of hi-tech, be mainly used in and make thick film integrated circuit, resistor, resistor network, electrical condenser, conductor ink, electrode of solar battery, printing and high resolving power electrical conductor, conductive resin, sensitive components and other electronic devices and components, also be widely used at industrial circles such as aviation, chemical industry, printing, building and military affairs.
Electrocondution slurry is used comparative maturity abroad, and since the sixties, successively there be more than 20 company's exploitation such as ESL, Englehard, Cermalley, Ferro, EMCA, Heraeus, IBM, Lei Qiesi, General Electric in the U.S., makes, and sells all kinds of electrocondution slurries.Europe production and sales slurry and raw-material company, famous have Degussa, a Philips etc.After the eighties, Japan develops into main in the world slurry producing country gradually, is unique slurry big country that can contend with the U.S..There are Sumitomo Metal Industries mine, clear flourish chemistry, Tanaka's precious metal institute, Murata Manufacturing Co. Ltd., TAIYO YUDAN, Hitachi chemical, Toshiba's chemistry, FUKUDA METAL's powder, Mitsubishi's metal, NEC, TDK etc. in famous slurry company.
China sets foot in electric slurry than later, mainly in the later stage eighties, is representative with Kunming precious metal and 4310 factories.About calendar year 2001, China's electric slurry development is wherein had outstanding performance with the slurry of the National University of Defense technology's sharp moral production in exploitation Hunan rapidly especially.Mainly based on conductor paste (silver slurry, aluminium-silver slurry), other slurries are used upward not yet in place in the application of China's electric slurry, and this mainly is that reason is cheaply pursued by China.
Electric slurry is as a kind of type material, and is excellent in far away traditional circuit equipment (as resistance wire, electrothermal tube etc.), and has environmental protection, characteristics such as efficient and energy-conservation, and its cost is also approaching with traditional material, will be main application direction in the future undoubtedly.
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.
The living environment of depending on for existence for the better maintaining mankind realizes continuous development of society economy, and numerous and confused formulation of developed country is fit to own environmental protection policy, and it is produced and the electronic product of import carries out environmental protection and limits.Japan takes the lead in initiating manufacturing leadless electronic product at the end of the nineties, now European Union is more executed with the law of strictness: European Union has announced " waste electronic andelectrical equipment instruction " (being called for short the WEEE instruction) and " about ban use of some objectionable impurities instruction in electronic electric equipment " (being called for short the RoHS instruction) of the common approval of European Parliament and the EU Council of Ministers on the L37 phase " Official Journal " in 2003, to reduce the influence of electronics contain hazardous substance to environment.Wherein RoHS instruction (Restrictionof Use of Hazardous Substances) is also referred to as " unleaded regulations ", and these regulations require 1 day July in 2006 after the electronic product in the regional list marketing of European Union must not exceed standard without exception to contain 6 kinds of objectionable impuritiess with headed by the lead.
China is constantly transferred in current main electronics manufacturing and design, the relevant government department of China responds actively the RoHS of European Union instruction, and announced Chinese version RoHS instruction in January, 2005, be contemplated for and implement in December, 2005, Chinese version RoHS and the version RoHS of European Union content are identical substantially, and its difference is that the device category that is limited will lack.European Union's version RoHS content meets the product that RoHS requires, any following substances content should satisfy: this substances content is no more than the maximum value of stipulating below in the homogeneous material, unless this material is the material that the RoHS instruction is exempted: plumbous (Pb), mercury (Hg), sexavalent chrome (Cr 6+), polymerization bromination connection stupid (PBB), and the polymerization bromination joins stupid ether (PBDE) content and is no more than 0.1% of gross weight, cadmium (Cd) content is no more than 0.01% of gross weight.
The USP of E.I.Du Pont Company 4537703 has proposed that a class is unleaded, the barium borosilicate glass of Chrome-free, is used to make the slurry of the thick-film resistor of 10～30 ohm of low-resistance values.The chief component of this thick-film resistor paste in conjunction with phase, i.e. the glass of this patent, play bonding conductive phase discrete particles film forming and with the effect of base plate bonding.This patent thinks that employing stannic oxide-tantalum tin pyrrhite matrix material is that to make the low resistance thick-film resistor be very strict to the requirement of glass to conductive phase.The characteristics that this patent glass is formed are: 1. glass network former SiO 2, B 2O 3, SnO 2Total amount 50%～85% molar percentage, wherein 20%～50% B 2O 3, 15%～40% SiO 2, 0.1%～5% SnO 2SnO 2Be to form, it is a glass-former, can reduce resistance again, but because SnO 2Solubleness is limited, and actual amount is no more than 4%; 2. network modification body total amount 15%～50%, 20%～50% BaO wherein, 2%～12% CoO, 1%～10% NiO.NiO must form, and can obtain suitable electrical resistance property.The sintering temperature of the slurry that the glass powder of this patent is made is at 800～900 ℃, and time 5～15min illustrates that this kind glass powder is suitable for high temperature sintering, can not be used for the electric slurry of low temperature or intermediate sintering temperature.
The US4362656 of E.I.Du Pont Company has disclosed a kind of ruthenium oxide base thick-film resistor paste glass powder, is characterized in that adhering glass is PbO-SiO 2And PbO-B 2O 3-SiO 2System owing to contain a large amount of lead (up to 65wt%) in this glass powder, therefore, does not meet environmental protection requirement.
[summary of the invention]
Main purpose of the present invention is to overcome the deficiency of existing electrocondution slurry with glass powder, a kind of electrocondution slurry lead-free glass powder and preparation method thereof is provided, have that sintering temperature is low, resistance to air loss and the good characteristics of chemical durability, particularly have good acid resistance.
The objective of the invention is to be achieved through the following technical solutions:
A kind of lead-free glass powder, raw materials by weight consists of:
SiO 2 30～50％
B 2O 3 1～10％
Al 2O 3 1～10％
BaO 1～20％
ZnO 1～10％
TiO 2 1～10％
Na 2O 1～20％
Li 2O 1～10％
ZrO 2 1～5％
V 2O 5 1～10％
Co 3O 4 0.1～2％；
Described SiO 2Be preferably 35～45%, the best is 42%;
Described B 2O 3Be preferably 3～9%, the best is 9%;
Described Al 2O 3Be preferably 3～5%, the best is 4%;
Described BaO is preferably 5～10%, and the best is 8%;
Described ZnO is preferably 3～7%, and the best is 6%;
Described TiO 2Be preferably 2～5%, the best is 4%;
Described Na 2O is preferably 5～15%, and the best is 14%;
Described Li 2O is preferably 3～8%, and the best is 5%;
Described ZrO 2Be preferably 1～3%, the best is 2%;
Described V 2O 5Be preferably 3～7%, the best is 5.5%;
Described Co 3O 4Be preferably 0.4～1%, the best is 0.5%;
Total weight percent of described ZnO/BaO is less than 1;
Described Na 2O, Li 2Total weight percent of O is 8～25%.
Another object of the present invention is to provide a kind of preparation method who is used for above-mentioned a kind of lead-free glass powder, 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 1300 ℃～1400 ℃ electric furnace, insulation 3～6h 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.
A kind of lead-free glass powder of the present invention and preparation method thereof with the positively effect of application in computer realm 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) of the present invention 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 of the present invention shows, not only has thermal expansivity suitable and that be easy to adjust, suitable softening temperature, also has excellent chemical stability, has very strong competitive power aspect unleaded and the excellent performance especially, have the high advantage of cost performance, have market development prospect widely;
(4) the final acid resistance of product 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]
Below by specific embodiment technical scheme of the present invention is described in detail.
Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
One, the raw material composition is by weight percentage:
SiO 2Be 42%, B 2O 3Be 9%, Al 2O 3Be 4%, BaO is 8%, and ZnO is 6%, TiO 2Be 4%, Na 2O is 14%, Li 2O is 5%, ZrO 2Be 2%, V 2O 5Be 5.5%, Co 3O 4Be 0.5%.
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 1360 ℃ 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:
The coefficient of expansion: 103 * 10 -7/ ℃ (300 ℃)
Sintering temperature: 630 ℃
Acid resistance:＜0.2wt% (5wt% sulfuric acid/3h).
Embodiment 2
One, the raw material composition is by weight percentage:
SiO 2Be 36%, B 2O 3Be 8%, Al 2O 3Be 3%, BaO is 14%, and ZnO is 8%, TiO 2Be 5%, Na 2O is 11%, Li 2O is 6%, ZrO 2Be 2%, V 2O 5Be 6.8%, Co 3O 4Be 0.2%.
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 1320 ℃ electric furnace, insulation 3h 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:
The coefficient of expansion: 98.7 * 10 -7/ ℃ (300 ℃)
Sintering temperature: 600 ℃
Acid resistance:＜0.2wt% (5wt% sulfuric acid/3h).
Embodiment 3
One, the raw material composition is by weight percentage:
SiO 2Be 40%, B 2O 3Be 10%, Al 2O 3Be 2%, BaO is 13%, and ZnO is 10%, TiO 2Be 4%, Na 2O is 12%, Li 2O is 4%, ZrO 2Be 1%, V 2O 5Be 3%, Co 3O 4Be 1%.
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 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:
The coefficient of expansion: 98.1 * 10 -7/ ℃ (300 ℃)
Sintering temperature: 610 ℃
Acid resistance:＜0.2wt% (5wt% sulfuric acid/3h).
Embodiment 4
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 9%, TiO 2Be 2%, Na 2O is 8%, Li 2O is 4%, ZrO 2Be 1%, V 2O 5Be 2%, Co 3O 4Be 1%.
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 1390 ℃ electric furnace, insulation 5h 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:
The coefficient of expansion: 77 * 10 -7/ ℃ (300 ℃)
Sintering temperature: 630 ℃
Acid resistance:＜0.2wt% (5wt% sulfuric acid/3h).
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 (10)

1. a lead-free glass powder is characterized in that raw materials by weight consists of: SiO 2Be 30～50%, B 2O 3Be 1～10%, Al 2O 3Be 1～10%, BaO is 1～20%, and ZnO is 1～10%, TiO 2Be 1～10%, Na 2O is 1～20%, Li 2O is 1～10%, ZrO 2Be 1～5%, V 2O 5Be 1～10%, Co 3O 4Be 0.1～2%.
2. a kind of lead-free glass powder as claimed in claim 1 is characterized in that, described SiO 2Be 35～45%, described B 2O 3Be 3～9%, described Al 2O 3Be 3～5%, described BaO is 5～10%.
3. a kind of lead-free glass powder as claimed in claim 2 is characterized in that, described SiO 2Be 42%, described B 2O 3Be 9%, described Al 2O 3Be 4%, described BaO is 8%.
4. a kind of lead-free glass powder as claimed in claim 1 is characterized in that, described ZnO is 3～7%, described TiO 2Be 2～5%, described Na 2O is 5～15%, described Li 2O is 3～8%.
5. a kind of lead-free glass powder as claimed in claim 4 is characterized in that, described ZnO is 6%, described TiO 2Be 4%, described Na 2O is 14%, described Li 2O is 5%.
6. a kind of lead-free glass powder as claimed in claim 1 is characterized in that, described ZrO 2Be 1～3%, described V 2O 5Be 3～7%, described Co 3O 4Be 0.4～1%.
7. a kind of lead-free glass powder as claimed in claim 6 is characterized in that, described ZrO 2Be 2%, described V 2O 5Be 5.5%, described Co 3O 4Be 0.5%.
8. a kind of lead-free glass powder as claimed in claim 1 is characterized in that, total weight percent of described ZnO/BaO is less than 1.
9. a kind of lead-free glass powder as claimed in claim 1 is characterized in that, described Na 2O, Li 2Total weight percent of O is 8～25%.
10. the preparation method of a kind of lead-free glass powder as claimed in claim 1 is characterized in that, comprises the steps:
(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 1300 ℃～1400 ℃ electric furnace, insulation 3～6h 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.
CN200910198372A 2009-11-06 2009-11-06 Lead-free glass powder and preparation method thereof and application thereof in computer field Pending CN101717197A (en)

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Application Number Priority Date Filing Date Title
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134157A (en) * 2011-04-15 2011-07-27 浙江高明玻璃有限公司 Lead-free low-melting-point glass powder and production process thereof
CN105731809A (en) * 2014-12-11 2016-07-06 北京有色金属研究总院 Insulating material for heating wire, preparation and application method thereof
CN107545946A (en) * 2017-08-21 2018-01-05 浙江安扬新能源科技有限公司 A kind of resistance slurry for stainless steel thick film circuit and preparation method thereof
CN110423013A (en) * 2019-08-27 2019-11-08 广东风华高新科技股份有限公司 A kind of copper electrocondution slurry glass powder, preparation method and application
CN112735716A (en) * 2020-12-23 2021-04-30 钢铁研究总院 Samarium-cobalt magnet glass coating with good wettability and preparation method thereof
CN114155992A (en) * 2021-11-29 2022-03-08 航天特种材料及工艺技术研究所 High-adhesion conductive silver paste for ceramic matrix composite and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134157A (en) * 2011-04-15 2011-07-27 浙江高明玻璃有限公司 Lead-free low-melting-point glass powder and production process thereof
CN102134157B (en) * 2011-04-15 2013-01-16 浙江高明玻璃有限公司 Lead-free low-melting-point glass powder and production process thereof
CN105731809A (en) * 2014-12-11 2016-07-06 北京有色金属研究总院 Insulating material for heating wire, preparation and application method thereof
CN107545946A (en) * 2017-08-21 2018-01-05 浙江安扬新能源科技有限公司 A kind of resistance slurry for stainless steel thick film circuit and preparation method thereof
CN110423013A (en) * 2019-08-27 2019-11-08 广东风华高新科技股份有限公司 A kind of copper electrocondution slurry glass powder, preparation method and application
CN112735716A (en) * 2020-12-23 2021-04-30 钢铁研究总院 Samarium-cobalt magnet glass coating with good wettability and preparation method thereof
CN114155992A (en) * 2021-11-29 2022-03-08 航天特种材料及工艺技术研究所 High-adhesion conductive silver paste for ceramic matrix composite and preparation method thereof

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Application publication date: 20100602