CN102173582A - Media glass used for infrared heating coating and preparation method thereof - Google Patents
Media glass used for infrared heating coating and preparation method thereof Download PDFInfo
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- CN102173582A CN102173582A CN 201110045936 CN201110045936A CN102173582A CN 102173582 A CN102173582 A CN 102173582A CN 201110045936 CN201110045936 CN 201110045936 CN 201110045936 A CN201110045936 A CN 201110045936A CN 102173582 A CN102173582 A CN 102173582A
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- medium glass
- infrared heating
- heating coating
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Abstract
The invention relates to a media glass used for infrared heating coating and a preparation method thereof. The media glass comprises the following components in percentage by weight: 40-65wt% of P2O5, 10-26wt% of ZnO, 14-32wt% of B2O3, 2-10wt% of Al2O3, 0-4wt% of Na2O, 0-4wt% of Li2O, 1-5wt% of CaO and 1-5wt% of MgO. The preparation method comprises the following steps: (1) evenly mixing components, melting in a silicon carbide rod electric furnace to obtain molten glass; and (2) shaping the molten glass in a preheated mould, annealing and cooling to process and shape the media glass. The media glass does not contain noble heavy metal or lead and is environmentally-friendly, the heat sealing temperature and the thermal expansion coefficient of glass are moderate, and the defects or shortages of the prior art are made up. The preparation method has the advantages of simple technology, low cost and good application prospect.
Description
Technical field
The invention belongs to the field of the medium glass of electronic devices and components, particularly a kind of medium glass that is used for the Infrared Heating coating and preparation method thereof.
Background technology
Plumbous oxide has very strong glass forming ability as a kind of low cost raw material.In field of electronic devices, leaded seal glass have preparation easily, melting temperature sealing is low, physical strength is high, good chemical stability, thereby be used widely.Although these leaded seal glasses use in commercial sealing-in, also there are many weak points, wherein the most tangible is exactly to contain in this glass HUMAN HEALTH and the deleterious PbO of environment.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.The phosphate system medium glass is as a kind of dielectric material that market outlook are arranged very much, has that melting temperature sealing is lower, the coefficient of expansion is easy to multiple advantages such as adjusting, is expected to replace traditional leaded seal glass.
The progress of current science and technology development, human society proposes higher requirement to seal, sealing materials, and melting temperature sealing is low, thermal expansivity a wider range, chemical stability dielectric material or seal, sealing materials good, reasonable price will be popular.Modern age microelectronics, electronics show and the advancing fast of photoelectron technology in, device miniaturization, structural element precise treatment have become main flow.Many technologies are more and more higher to the resistance to air loss and the reliability of sealing-in goods, require to reduce as far as possible melting temperature sealing when optimizing the preparation technology of photoelectron, microelectronic device.But reducing melting temperature sealing simply will cause the composite bed chemical stability to reduce, the medium bonding strength descends, and make the coefficient of expansion of dielectric material too big, if the coefficient of expansion of glass is too big, then the coefficient of expansion matching problem between itself and body material also will be difficult to solve.
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 ZrO
2Content higher, therefore aspect cost, do not have advantage equally.
United States Patent (USP) has been announced a kind of phosphate seal glass No. 5153151, 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 molecular fraction that H7-69672 number disclosed glass of Japanese Patent is formed is: P
2O
525～50%, SnO 30～70%, and ZnO 0～25%, add an amount of B on this basis
2O
3, WO
3, Li
2O etc.SnO/ZnO during the glass of this system is formed was greater than 5: 1, and the use temperature of glass is 350～450 ℃, and thermal expansivity is greater than 120 * 10
-7/ ℃, the method for employing weighting agent reduces the coefficient of expansion, the flowability the when adding of weighting agent has influence on glass sealing and the resistance to air loss of sealing device of glass in the patent.
Summary of the invention
Technical problem to be solved by this invention provides a kind of medium glass that is used for the Infrared Heating coating and preparation method thereof, the not leaded noble metal that do not contain of this medium glass, the oxide compound of all composition glass is abundant at occurring in nature content, environmental friendliness, the melting temperature sealing and the thermal expansivity of glass are moderate, and being suitable for alumina-ceramic, vehicle glass, No. ten materials such as stainless steel is the Infrared Heating device of substrate; Preparation method's technology is simple, and cost is low, has a good application prospect.
A kind of medium glass that is used for the Infrared Heating coating of the present invention, its component comprises: by weight percentage, 40～65%P
2O
5, 10～26%ZnO, 14～32%B
2O
3, 2～10%Al
2O
3, 0～4%Na
2O, 0～4%Li
2O, 1～5%CaO and 1～5%MgO.
Described medium glass component comprises, by weight percentage, and 45～57%P
2O
5, 13～22.5%ZnO, 18～22%B
2O
3, 2～5%Al
2O
3, 0.5～2.5%Na
2O, 0.5～3%Li
2O, 2～4%CaO and 3～4.5%MgO.
P in the described medium glass component
2O
5And B
2O
3Total weight percent be 55～75%.
Na in the described medium glass component
2O and Li
2The total weight percent of O is 1～6%.
The total weight percent of CaO and MgO is 2～6% in the described medium glass component.
Described medium glass thermal expansivity is 80～100 * 10
-7/ ℃.
Described medium glass transition temperature is 420～460 ℃, and softening temperature is 470～530 ℃.
A kind of preparation method who is used for the medium glass of Infrared Heating coating of the present invention comprises:
(1) by weight percentage, with 40～65%P
2O
5, 10～26%ZnO, 14～32%B
2O
3, 2～10%Al
2O
3, 0～4%Na
2O, 0～4%Li
2O, 1～5%CaO and 1～5%MgO mix, and are melted into glass metal in the globars electric furnace, and glass melting temperature is 1050～1220 ℃, are incubated 0.5～1.5 hour; In 200～500 ℃, heat-up rate is 2～3 ℃/min, and the heat-up rate that all the other temperature ranges (25～200 ℃, 500～1220 ℃) adopt is 5～10 ℃/min;
(2) with the die for molding of the above-mentioned glass metal that melts in the process preheating, anneal then, annealing temperature is 380～420 ℃, is incubated 1 hour postcooling, and last machine-shaping gets medium glass.
P in the described step (1)
2O
5Raw material is an ammonium phosphate, B
2O
3Raw material is a boric acid, Al
2O
3Raw material is an aluminium hydroxide, Na
2O, Li
2The raw material of O, CaO and MgO is each self-corresponding carbonate.
P in the medium glass component
2O
5And B
2O
3Be glass-former, form good vitreous state in order to guarantee glass, weight percent must reach 55～75%, P
2O
5Content significantly greater than B
2O
3Content, this is in order to reduce by two phase mutual interference between the organizer, reduces the unstable of glass system, thereby reduces the phase-splitting of glass system or the probability of crystallization.
Add Na in the medium glass component
2O and Li
2O is in order to strengthen glass forming ability, to make glass system more stable, adopting two alkali Na
2O and Li
2O is the two alkali effects that utilize in the glass, the physicalies such as thermal expansivity, resistivity and chemical stability of better feed glass, and also in order to make two alkali effects maximizations, the content of two alkali is preferably close in the glass.
Add CaO and MgO in the medium glass component on the one hand in order to strengthen glass forming ability, but the more important thing is the thermal expansivity of feed glass, making it to be suitable for thermal expansivity is 80～100 * 10
-7/ ℃ the substrate of heating coating, add MgO and be thermal expansivity for the glass of being more convenient for.
Principle of the present invention is: form good vitreous state in order to guarantee glass, reduce glass phase-splitting or tendency towards devitrification, P
2O
5And B
2O
3Content reaches 55～70%, adds the ZnO about 20%, forms the TERNARY GLASS system; Al
2O
3Adding be in order to make glass system more stable; Add Na in the glass ingredient
2O and Li
2O is in order to regulate the formation ability and the coefficient of expansion of glass, more can to utilize the two alkali effects in the glass to improve glass properties; Add CaO and MgO in the glass ingredient, in order to strengthen glass forming ability, the thermal expansivity of feed glass; Add Na in the glass
2O and Li
2O belongs to coarse adjustment, adds CaO and MgO and belongs to fine setting.
Beneficial effect
(1) the not leaded noble metal that do not contain of the present invention, the oxide compound of all composition glass is abundant at occurring in nature content, environmental friendliness, the melting temperature sealing and the thermal expansivity of glass are moderate, remedied the deficiencies in the prior art or defective, being suitable for alumina-ceramic, vehicle glass, No. ten materials such as stainless steel is the Infrared Heating device of substrate;
(2) preparation method's technology is simple, and cost is low, has a good application prospect.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.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
57%P by weight percentage
2O
5, 13%ZnO, 18%B
2O
3, 4%Al
2O
3, 1%Na
2O, 1%Li
2O, 3%CaO and 3%MgO prepare burden, and the glass compound is placed in the quartz crucible, found at globars electric furnace internal heating, and in 200～500 ℃, the heat-up rate of employing is 2～3 ℃/min; All the other temperature ranges (25～200 ℃, 500～1180 ℃) adopt being rapidly heated of 5～10 ℃/min, to 1180 ℃ of insulation 60min;
The glass metal that melts is through the die for molding of preheating, and puts into retort furnace fast and anneal, and annealing temperature is 420 ℃, is incubated furnace cooling after 1 hour;
Sample after the annealing carries out performance analysis after attrition process, test result sees Table 1.
Embodiment 2
50%P by weight percentage
2O
5, 20%ZnO, 21%B
2O
3, 2%Al
2O
3, 1%Na
2O, 1%Li
2O, 2%CaO and 3%MgO prepare burden, and the glass compound is placed in the quartz crucible, found at globars electric furnace internal heating, and in 200～500 ℃, the heat-up rate of employing is 2～3 ℃/min; All the other temperature ranges (25～200 ℃, 500～1180 ℃) adopt being rapidly heated of 5～10 ℃/min, to 1180 ℃ of insulation 60min.
The glass metal that melts is through the die for molding of preheating, and puts into retort furnace fast and anneal, and annealing temperature is 420 ℃, is incubated furnace cooling after 1 hour.
Sample after the annealing carries out performance analysis after attrition process, test result sees Table 1.
Embodiment 3
45%P by weight percentage
2O
5, 22.5%ZnO, 18%B
2O
3, 5%Al
2O
3, 0.5%Na
2O, 0.5%Li
2O, 4%CaO and 4.5%MgO prepare burden, and the glass compound is placed in the quartz crucible, found at globars electric furnace internal heating, and in 200～500 ℃, the heat-up rate of employing is 2～3 ℃/min; All the other temperature ranges (25～200 ℃, 500～1220 ℃) adopted being rapidly heated of 5～10 ℃/min, to 1220 ℃ of insulations 1.5 hours.
The glass metal that melts is through the die for molding of preheating, and puts into retort furnace fast and anneal, and annealing temperature is 380 ℃, is incubated furnace cooling after 1 hour.
Sample after the annealing carries out performance analysis after attrition process, test result sees Table 1.
Embodiment 4
47%P by weight percentage
2O
5, 14%ZnO, 22%B
2O
3, 3%Al
2O
3, 2.5%Na
2O, 3%Li
2O, 4%CaO and 4.5%MgO prepare burden, and the glass compound is placed in the quartz crucible, found at globars electric furnace internal heating, and in 200～500 ℃, the heat-up rate of employing is 2～3 ℃/min; All the other temperature ranges (25～200 ℃, 500～1150 ℃) adopt being rapidly heated of 5～10 ℃/min, to 1150 ℃ of insulation 50min.
The glass metal that melts is through the die for molding of preheating, and puts into retort furnace fast and anneal, and annealing temperature is 420 ℃, is incubated furnace cooling after 1 hour.
Sample after the annealing carries out performance analysis after attrition process, test result sees Table 1.
Table 1 is used for the performance of the medium glass of Infrared Heating coating
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| α(×10 -7/℃) | 85.6 | 83.6 | 89.1 | 92.2 |
| Transition temperature Tg ℃) | 447 | 444 | 457 | 436 |
| Softening temperature Tf (℃) | 492 | 485 | 506 | 468 |
Claims (9)
1. medium glass that is used for the Infrared Heating coating, its component comprises: by weight percentage, 40～65%P
2O
5, 10～26%ZnO, 14～32%B
2O
3, 2～10%Al
2O
3, 0～4%Na
2O, 0～4%Li
2O, 1～5%CaO and 1～5%MgO.
2. a kind of medium glass that is used for the Infrared Heating coating according to claim 1 is characterized in that: described medium glass component comprises, by weight percentage, and 45～57%P
2O
5, 13～22.5%ZnO, 18～22%B
2O
3, 2～5%Al
2O
3, 0.5～2.5%Na
2O, 0.5～3%Li
2O, 2～4%CaO and 3～4.5%MgO.
3. a kind of medium glass that is used for the Infrared Heating coating according to claim 1 is characterized in that: P in the described medium glass component
2O
5And B
2O
3Total weight percent be 55～75%.
4. a kind of medium glass that is used for the Infrared Heating coating according to claim 1 is characterized in that: Na in the described medium glass component
2O and Li
2The total weight percent of O is 1～6%.
5. a kind of medium glass that is used for the Infrared Heating coating according to claim 1 is characterized in that: the total weight percent of CaO and MgO is 2～6% in the described medium glass component.
6. a kind of medium glass that is used for the Infrared Heating coating according to claim 1 is characterized in that: described medium glass thermal expansivity is 80～100 * 10
-7/ ℃.
7. a kind of medium glass that is used for the Infrared Heating coating according to claim 1 is characterized in that: described medium glass transition temperature is 420～460 ℃, and softening temperature is 470～530 ℃.
8. preparation method who is used for the medium glass of Infrared Heating coating comprises:
(1) by weight percentage, with 40～65%P
2O
5, 10～26%ZnO, 14～32%B
2O
3, 2～10%Al
2O
3, 0～4%Na
2O, 0～4%Li
2O, 1～5%CaO and 1～5%MgO mix, and are melted into glass metal in the globars electric furnace, and glass melting temperature is 1050～1220 ℃, are incubated 0.5～1.5 hour; In 200～500 ℃, heat-up rate is 2～3 ℃/min, and the heat-up rate that all the other temperature ranges adopt is 5～10 ℃/min;
(2) with the die for molding of the above-mentioned glass metal that melts in the process preheating, anneal then, annealing temperature is 380～420 ℃, is incubated 1 hour postcooling, and last machine-shaping gets medium glass.
9. a kind of preparation method who is used for the medium glass of Infrared Heating coating according to claim 8 is characterized in that: P in the described step (1)
2O
5Raw material is an ammonium phosphate, B
2O
3Raw material is a boric acid, Al
2O
3Raw material is an aluminium hydroxide, Na
2O, Li
2The raw material of O, CaO and MgO is each self-corresponding carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110045936 CN102173582A (en) | 2011-02-25 | 2011-02-25 | Media glass used for infrared heating coating and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110045936 CN102173582A (en) | 2011-02-25 | 2011-02-25 | Media glass used for infrared heating coating and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102173582A true CN102173582A (en) | 2011-09-07 |
Family
ID=44516881
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110045936 Pending CN102173582A (en) | 2011-02-25 | 2011-02-25 | Media glass used for infrared heating coating and preparation method thereof |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584012A (en) * | 2012-02-10 | 2012-07-18 | 南通南京大学材料工程技术研究院 | Low-melting-point optical glass and preparation method thereof |
| CN115448600A (en) * | 2022-10-28 | 2022-12-09 | 江西科技师范大学 | Boron aluminate microcrystalline glass and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1754851A (en) * | 2004-09-29 | 2006-04-05 | Hoya株式会社 | Phosphate optical glass, preform for precise press molding and method of manufacturing the same, optical device and method of manufacturing the same |
| CN1807313A (en) * | 2006-01-10 | 2006-07-26 | 陕西科技大学 | Preparation method of foam glass |
| CN1830856A (en) * | 2006-03-17 | 2006-09-13 | 东华大学 | Leadless phosphate seal glass and its preparation method |
-
2011
- 2011-02-25 CN CN 201110045936 patent/CN102173582A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1754851A (en) * | 2004-09-29 | 2006-04-05 | Hoya株式会社 | Phosphate optical glass, preform for precise press molding and method of manufacturing the same, optical device and method of manufacturing the same |
| CN1807313A (en) * | 2006-01-10 | 2006-07-26 | 陕西科技大学 | Preparation method of foam glass |
| CN1830856A (en) * | 2006-03-17 | 2006-09-13 | 东华大学 | Leadless phosphate seal glass and its preparation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584012A (en) * | 2012-02-10 | 2012-07-18 | 南通南京大学材料工程技术研究院 | Low-melting-point optical glass and preparation method thereof |
| CN115448600A (en) * | 2022-10-28 | 2022-12-09 | 江西科技师范大学 | Boron aluminate microcrystalline glass and preparation method thereof |
| CN115448600B (en) * | 2022-10-28 | 2023-11-10 | 江西科技师范大学 | Boron aluminate microcrystalline glass and preparation method thereof |
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Application publication date: 20110907 |