CN101708956A - Low melting-point glass powder for field of computers and preparation method thereof - Google Patents

Low melting-point glass powder for field of computers and preparation method thereof Download PDF

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Publication number
CN101708956A
CN101708956A CN200910198374A CN200910198374A CN101708956A CN 101708956 A CN101708956 A CN 101708956A CN 200910198374 A CN200910198374 A CN 200910198374A CN 200910198374 A CN200910198374 A CN 200910198374A CN 101708956 A CN101708956 A CN 101708956A
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glass powder
low melting
melting point
percent
glass
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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 provides a low melting-point glass powder for the field of computers and a preparation method thereof. The low melting-point glass powder comprises the following raw materials in percentage by weight: 30 to 50 percent of V205, 5 to 30 percent of P205, 1 to 20 percent of ZnO, 1 to 20 percent of B2O3, 1 to 10 percent of Al2O3, 1 to 10 percent of BaO, 1 to 10 percent of MnO2, 1 to 10 percent of SrO, 1 to 10 percent of TiO2 and 1 to 10 percent of Sb2O3. The preparation method comprises the following steps of: weighing, mixing, melting, tabletting, ball milling and sieving. The low melting-point glass powder has the following advantages of low softening temperature, wide adjustable range for expansion coefficient, good chemical stability and electrical performance, excellent fluidity and the like. The preparation method is suitable for encapsulating a plurality of electronic elements for the computer and for encapsulating high-power tubes, relay sockets and the like. Furthermore, the preparation method has excellent encapsulation airtightness.

Description

A kind of glass powder with low melting point that is used for computer realm and preparation method thereof
[technical field]
The invention belongs to field of computer technology, glass powder with low melting point of particularly a kind of electronic component sealing-in that is used for computer realm and preparation method thereof.
[background technology]
Existing computer electronic component is commonly used to low-melting sealing glass, in low-melting sealing glass, leaded seal glass has series of characteristics such as resistance is big, dielectric loss is little, specific refractory power and chromatic dispersion height and absorption high-energy radiation, softening temperature is low, chemical stability is good, and purposes is widely being arranged aspect the eutectic sealing-in.
Because great majority are flint glass in the commercial seal glass that uses at present, lead is very harmful to human body and environment.American-European, day has all formulated the unleaded mandatory implementation date of electronic product.China Ministry of Information Industry has also issued relevant regulations.Therefore, the successful exploitation of nuisanceless low-melting point sealing glass such as lead-free and cadmium-free will form the product technology barrier, the industry face that it relates to is very extensive, consumption is big, and industries such as China's household electrical appliances, precision parts, 3C (computer, communication, consumer electronics product) electronic product are had crucial strategic importance.
Enhancing day by day along with human environmental consciousness; plumbous by environmental protection institution list in preceding 17 kinds to one of human and chemical substance that environmental hazard is very big; 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.The intravital lead of people mainly enters human body from food or through the form of lead fume and lead dust by respiratory tract.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 the whole body organ by blood and tissue is gone 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.Chronic lead poisoning is only felt tired at first, loses the appetite, is lost weight etc.When chronic poisoning develops again, will present headache, tinnitus, visual disorder, miscarriage, anaemia, psychiatric disorder, early wait indefinitely.Therefore, ban use of the cry of leaded material more and more higher on a large scale.Plumbous use in drinking water pipeline welding, gasoline, oil painting early has strict regulation.Now in the electron trade round Realization not have the needs of leaded joint more and more urgent, whole industry is formed huge impact.In recent years, along with microelectronics, electronics show, the development of photoelectron technology.Requirement to the performance of sealing-in goods and technology is more and more higher, also makes the seal glass industry obtain certain development.The research of China aspect seal glass also has certain distance with Japan, Korea S, America and Europe.
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 (Restriction of 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.
People's such as the Beall of Corning Incorporated USP5122484 has proposed a class R 2O-ZnO-P 2O 5System's low melting glass, its weight percent is: P 2O 5(38-50%), MoO 3(0-10%), Al 2O 3(0-5%), WO 3(0-10%), Na 2O (2-10%), Li 2O (0.75-5%), SnO (0-10%), K 2O (2-10%), Cl (0-8%), the form with NaCl in the composition is introduced Cl, and the adding of chlorine significantly increases the flowability of glass, but NaCl loss 50-70% when fusing, WO 3Introducing also be increase mobile.Above-mentioned glass sealing temperature is lower than 475 ℃, and coefficient of expansion α is (100-105) * 10 -7/ ℃, for reducing the coefficient of expansion, can add weighting agent, the deficiency of above-mentioned seal glass is that chemical stability is bad, particularly aspect the acid resistance or under the environment in humidity, flowability and resistance to air loss when influencing glass sealing during absorb fillers in addition.
The special fair 7-108786 of Germany Carl Zeiss Inc. patent proposes to contain the ZnO-PbO-B of CuO 2O 3-SiO 2System glass ceramics, be used for airtight sealing zinc oxide ceramics voltage dependent resistor, seal temperature＜540 ℃, in order to prevent the deterioration of this voltage dependent resistor current-voltage character, surperficial airtight sealing to be stoped atmosphere, water etc., this patent use properties excellence, but contain more lead (about 45%), can not satisfy the requirement of the feature of environmental protection.
U.S. Pat P:20020019303 has proposed a kind of seal glass of phosphor tin Zn system, 430 ℃～500 ℃ of sealing temperatures, owing to need under reducing atmosphere, produce and sealing-in, 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.
[summary of the invention]
Main purpose of the present invention is to overcome the deficiency of existing electronic component sealing-in glass powder with low melting point, a kind of glass powder with low melting point that is used for the sealing-in of computer electronic component and preparation method thereof is provided, glass powder with low melting point of the present invention is not leaded, can keep realizing the unleaded of electronic component sealing-in under the lower glass transition temperature, have that softening temperature is low, coefficient of expansion adjustable range big, advantages such as chemical stability and good electrical property, good fluidity.Be suitable for the sealing-in of multiple computer electronic component, and high power valve, the sealing-in of relay socket etc. has good sealing-in resistance to air loss.
The objective of the invention is to be achieved through the following technical solutions:
A kind of glass powder with low melting point that is used for computer realm, raw materials by weight consists of: V 2O 5Be 30～50%, P 2O 5Be 5～30%, ZnO is 1～20%, B 2O 3Be 1～20%, Al 2O 3Be 1～10%, BaO is 1～10%, MnO 2Be 1～10%, SrO is 1～10%, TiO 2Be 1～10%, Sb 2O 3Be 1～10%;
Described V 2O 5Be preferably 35～45%, the best is 44%;
Described P 2O 5Be preferably 10～25%, the best is 18%;
Described ZnO is preferably 3～15%, and the best is 8%;
Described B 2O 3Be preferably 3～15%, the best is 9%;
Described Al 2O 3Be preferably 2～7%, the best is 3%;
Described BaO is preferably 2～7%, and the best is 5%;
Described MnO 2Preferred 2～7%, the best is 3%;
Described SrO is preferably 1～5%, and the best is 2%;
Described TiO 2Be preferably 1～5%, the best is 4%;
Described Sb 2O 3Be preferably 2～7%, the best is 4%;
Described Al 2O 3, MnO 2And TiO 2Total weight percent be 5～20%.
Another object of the present invention is to provide a kind of preparation method who is used for the glass powder with low melting point of computer realm, 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 1000 ℃～1200 ℃ electric furnace, insulation 50～150min;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours in the cold water or be cast into certain shape;
(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 glass powder with low melting point that is used for computer realm of the present invention is applied widely, except being applied to the sealing-in of computer electronic component, simultaneously can also with the glass that conforms to the coefficient of expansion in this temperature, pottery, metal sealing, sealing property is good.
The positively effect of a kind of glass powder with low melting point that is used for computer realm of the present invention and preparation method thereof 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.
A kind of glass powder with low melting point that is used for computer realm of the present invention not only has thermal expansivity suitable and that be easy to adjust, suitable softening temperature, also has excellent chemical stability, special in having very strong competitive power aspect unleaded and the excellent performance, have market development prospect widely.
[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.
The invention provides a kind of glass powder with low melting point that is widely used in computer realm, have low melting point, nontoxic, free of contamination advantage, to satisfy the demand of market the glass powder with low melting point of electronic component sealing-in.
A kind of glass powder with low melting point that is used for computer realm of the present invention, raw materials by weight consists of: V 2O 5Be 30～50%, P 2O 5Be 5～30%, ZnO is 1～20%, B 2O 3Be 1～20%, Al 2O 3Be 1～10%, BaO is 1～10%, MnO 2Be 1～10%, SrO is 1～10%, TiO 2Be 1～10%, Sb 2O 3Be 1～10%;
Described V 2O 5Be preferably 35～45%, the best is 44%;
Described P 2O 5Be preferably 10～25%, the best is 18%;
Described ZnO is preferably 3～15%, and the best is 8%;
Described B 2O 3Be preferably 3～15%, the best is 9%;
Described Al 2O 3Be preferably 2～7%, the best is 3%;
Described BaO is preferably 2～7%, and the best is 5%;
Described MnO 2Preferred 2～7%, the best is 3%;
Described SrO is preferably 1～5%, and the best is 2%;
Described TiO 2Be preferably 1～5%, the best is 4%;
Described Sb 2O 3Be preferably 2～7%, the best is 4%;
Described Al 2O 3, MnO 2And TiO 2Total weight percent be 5～20%.
A kind of glass powder with low melting point that is used for computer realm of the present invention is applied widely, except being applied to the sealing-in of computer electronic component, simultaneously can also with the glass that conforms to the coefficient of expansion in this temperature, pottery, metal sealing, sealing property is good.
A kind of glass powder with low melting point that is used for computer realm of the present invention not only has thermal expansivity suitable and that be easy to adjust, suitable softening temperature, also has excellent chemical stability, special in having very strong competitive power aspect unleaded and the excellent performance, have market development prospect widely.
Embodiment 1
One, the raw material composition is by weight percentage:
V 2O 5Be 44%, P 2O 5Be 18%, ZnO is 8%, B 2O 3Be 9%, Al 2O 3Be 3%, BaO is 5%, MnO 2Be 3%, SrO is 2%, TiO 2Be 4%, Sb 2O 3Be 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 1100 ℃ electric furnace, insulation 50min;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours in the cold water or be cast into certain shape;
(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:
Tg(℃)：＜300℃
Tf(℃)：＜400℃
The coefficient of expansion: 98 * 10 -7/ ℃ (300 ℃)
Water tolerance: good.
Embodiment 2
One, the raw material composition is by weight percentage:
V 2O 5Be 31%, P 2O 5Be 25%, ZnO is 8%, B 2O 3Be 15%, Al 2O 3Be 4%, BaO is 6%, MnO 2Be 2%, SrO is 1%, TiO 2Be 5%, Sb 2O 3Be 3%.
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 1200 ℃ electric furnace, insulation 140min;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours in the cold water or be cast into certain shape;
(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:
Tg(℃)：＜300℃
Tf(℃)：＜400℃
The coefficient of expansion: 92 * 10 -7/ ℃ (300 ℃)
Water tolerance: good.
Embodiment 3
One, the raw material composition is by weight percentage:
V 2O 5Be 40%, P 2O 5Be 18%, ZnO is 8%, B 2O 3Be 10%, Al 2O 3Be 4%, BaO is 9%, MnO 2Be 4%, SrO is 2%, TiO 2Be 3%, Sb 2O 3Be 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 1100 ℃ electric furnace, insulation 75min;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours in the cold water or be cast into certain shape;
(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:
Tg(℃)：＜300℃
Tf(℃)：＜400℃
The coefficient of expansion: 94 * 10 -7/ ℃ (300 ℃)
Water tolerance: good.
Embodiment 4
One, the raw material composition is by weight percentage:
V 2O 5Be 45%, P 2O 5Be 16%, ZnO is 6%, B 2O 3Be 12%, Al 2O 3Be 3%, BaO is 8%, MnO 2Be 3%, SrO is 2%, TiO 2Be 4%, Sb 2O 3Be 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 1120 ℃ electric furnace, insulation 100min;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours in the cold water or be cast into certain shape;
(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:
Tg(℃)：＜300℃
Tf(℃)：＜400℃
The coefficient of expansion: 99 * 10 -7/ ℃ (300 ℃)
Water tolerance: good.
Embodiment 5
One, the raw material composition is by weight percentage:
V 2O 5Be 50%, P 2O 5Be 15%, ZnO is 3%, B 2O 3Be 12%, Al 2O 3Be 2%, BaO is 5%, MnO 2Be 2%, SrO is 3%, TiO 2Be 5%, Sb 2O 3Be 3%.
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 1020 ℃ electric furnace, insulation 110min;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours in the cold water or be cast into certain shape;
(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:
Tg(℃)：＜300℃
Tf(℃)：＜400℃
The coefficient of expansion: 103 * 10 -7/ ℃ (300 ℃)
Water tolerance: good.
It should be noted that, the present invention can provide a kind of glass powder with low melting point that is used for computer realm that matches according to the characteristic of concrete seal, sealing materials and to the specific requirement of the temperature and the coefficient of expansion, obtains multiple a kind of glass powder with low melting point that is used for computer realm with different coefficients of expansion thereby its method is to select for use different components to constitute glass.
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. a glass powder with low melting point that is used for computer realm is characterized in that, the component that raw materials by weight is formed is V 2O 5Be 30～50%, P 2O 5Be 5～30%, ZnO is 1～20%, B 2O 3Be 1～20%, Al 2O 3Be 1～10%, BaO is 1～10%, MnO 2Be 1～10%, SrO is 1～10%, TiO 2Be 1～10%, Sb 2O 3Be 1～10%.
2. a kind of glass powder with low melting point that is used for computer realm as claimed in claim 1 is characterized in that described V 2O 5Be 35～45%; Described P 2O 5Be 10～25%; Described ZnO is 3～15%; Described B 2O 3Be 3～15%.
3. a kind of glass powder with low melting point that is used for computer realm as claimed in claim 2 is characterized in that described V 2O 5Be 44%; Described P 2O 5Be 18%; Described ZnO is 8%; Described B 2O 3Be 9%.
4. a kind of glass powder with low melting point that is used for computer realm as claimed in claim 1 is characterized in that described Al 2O 3Be 2～7%; Described BaO is 2～7%; Described MnO 2Be 2～7%.
5. a kind of glass powder with low melting point that is used for computer realm as claimed in claim 4 is characterized in that described Al 2O 3Be 3%; Described BaO is 5%; Described MnO 2Be 3%.
6. a kind of glass powder with low melting point that is used for computer realm as claimed in claim 1 is characterized in that described SrO is 1～5%; Described TiO 2Be 1～5%; Described Sb 2O 3Be 2～7%.
7. a kind of glass powder with low melting point that is used for computer realm as claimed in claim 6 is characterized in that described SrO is 2%; Described TiO 2Be 4%; Described Sb 2O 3Be 4%.
8. a kind of glass powder with low melting point that is used for computer realm as claimed in claim 1 is characterized in that described Al 2O 3, MnO 2And TiO 2Total weight percent be 5～20%.
9. a kind of preparation method who is used for the glass powder with low melting point of computer realm 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 1000 ℃～1200 ℃ electric furnace, insulation 50～150min;
(4) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours in the cold water or be cast into certain shape;
(5) sheet or granular glass are put into the ball mill ball milling;
(6) glass powder behind the ball milling is sieved, detects, packs.
CN200910198374A 2009-11-06 2009-11-06 Low melting-point glass powder for field of computers and preparation method thereof Pending CN101708956A (en)

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Application Number Priority Date Filing Date Title
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173593A (en) * 2011-02-12 2011-09-07 刘国正 Lead-free glass powder, preparation method and application thereof
CN104045235A (en) * 2013-03-12 2014-09-17 博思株式会社 Glass Frit Composition, Glass Frit Composition, And Sealing Method Of Amoled
CN104150778A (en) * 2014-08-11 2014-11-19 海南中航特玻材料有限公司 Lead-free and low-melting-point sealing glass
CN109184486A (en) * 2012-05-31 2019-01-11 佳殿工业公司 The method for preparing vacuum insulated glass building window unit

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173593A (en) * 2011-02-12 2011-09-07 刘国正 Lead-free glass powder, preparation method and application thereof
CN102173593B (en) * 2011-02-12 2013-03-27 刘国正 Lead-free glass powder, preparation method and application thereof
CN109184486A (en) * 2012-05-31 2019-01-11 佳殿工业公司 The method for preparing vacuum insulated glass building window unit
CN104045235A (en) * 2013-03-12 2014-09-17 博思株式会社 Glass Frit Composition, Glass Frit Composition, And Sealing Method Of Amoled
CN104045235B (en) * 2013-03-12 2016-11-16 博思株式会社 Glass frit compositions, frit and active matrix organic light-emitting diode Sealing Method
CN104150778A (en) * 2014-08-11 2014-11-19 海南中航特玻材料有限公司 Lead-free and low-melting-point sealing glass

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Application publication date: 20100519