CN105481414A - Low-stress alumina ceramic metal sealing method - Google Patents
Low-stress alumina ceramic metal sealing method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
- C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/612—Machining
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/12—Metallic interlayers
- C04B2237/123—Metallic interlayers based on iron group metals, e.g. steel
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Abstract
The present invention is a low-stress alumina ceramic metal sealing method, comprising the following steps: a) preparing of an alumina ceramic; 2) producing of a metalization pattern; 3) hot cutting; 4) high-temperature sintering; 5) preparation of an intermediate layer plating solution; 6) plating; 7) pre-treatment of a metal lead wire and a solder sheet; and 8) rack loading and brazing. Advantages are that Rockwell hardness of the metal lead wire is reduced to 80 or less, an alumina burnt ceramic tungsten metalization layer is coated with a nickel layer with thickness of 0.02 mum-5mum to ensure that the high barrier property of the intermediate layer in the brazing process, after sealing, the alumina ceramic and the metal lead wire are in a strength security stress state, the bonding strength is 8Kg / cm<2> or more, the alumina ceramic and metal lead wire sealing bonding strength and long-term reliability of a produced housing can meet the packaging requirements of digital circuits, microwave, power electronics, optoelectronics devices and other multilayer alumina ceramic housings, the process is simple, required production equipment is less, and industrial and low-cost mass production can be achieved.
Description
Technical field
The present invention is a kind of highly reliable high bond strength low-stress alumina-ceramic metal sealing method, be the manufacture method for encapsulation digital circuit, microwave, power electronics, photoelectric device and other multilayer alumina ceramic envelope, belong to technical field of electronic encapsulation.
Background technology
Multi-layer ceramic package shell because its structural strength is high, chemical stability is good, wiring density is high, electric heating property and microwave property excellent, be widely applied in fields such as communication, aerospace, automobile and consumer electronicses.In the last few years with large-scale integrated circuit to high frequency, highly reliable, multi-functional, miniaturization and lightweight future development, digital circuit, mimic channel, photoelectricity etc. are integrated on same device by increasing application requiring, linear density increase is walked in encapsulated circuit inside, inside and outside pin width between centers is reduced to 0.5mm from 1.27mm, 0.8mm, 0.65mm, even less, number of pins is increased to 1152 equal-specifications from 32, and packaging density increases.Metal lead wire wherein as shell input/output terminal plays a part microwave, electric transmission channel in device circuitry, the bonding strength of it and multilayer ceramic largely determines the reliability of device, therefore, obtaining highly reliable, high bond strength, low-stress alumina-ceramic metal sealing is the important guarantee realizing digital circuit, microwave, power electronics, photoelectric device and other multilayer alumina-ceramic packaging excellent signal transmission performances.
Summary of the invention
What the present invention proposed is a kind of highly reliable high bond strength low-stress alumina-ceramic metal sealing method, be the manufacture method for encapsulation digital circuit, microwave, power electronics, photoelectric device and other multilayer alumina ceramic envelope, for highly reliable, high bond strength, the low-stress sealing-in of digital circuit, microwave, power electronics, photoelectric device and other multilayer alumina-ceramic packagings pottery and metal lead wire.
Technical solution of the present invention: low-stress alumina-ceramic metal sealing method, comprises the steps:
1) alumina-ceramic is prepared;
2) metallization pattern makes;
3) fervent;
4) high temperature sintering;
5) middle layer plating solution is prepared;
6) plating;
7) metal lead wire and solder sheet pre-treatment;
8) soldering is shelved.
Advantage of the present invention: metal lead wire Rockwell hardness is reduced to less than 80, on aluminum oxide ripe porcelain tungsten metallization layer, nickel coating layer thickness is 0.02 μm ~ 5 μm, ensure that the high barrier in brazing process middle layer, good wetting property and free-running property, sealing-in rear oxidation aluminium pottery and metal lead wire are in the stressed condition of Strength Safety, and bonding strength brings up to 8Kg/cm
2and more than, at least improve 30% than traditional method, reliability improves 20%.According to the shell that operational path of the present invention and method make, its alumina-ceramic and metal lead wire sealing-in bonding strength and long-term reliability can meet the package requirements of digital circuit, microwave, power electronics, photoelectric device and other multilayer alumina ceramic envelope, have preparation technology's production unit that is simple, that need few, can the feature such as industrialization, low cost scale operation.
Accompanying drawing explanation
Fig. 1 is low-stress alumina-ceramic metal sealing process schema.
Fig. 2 is metallization alumina-ceramic intervening layers thickness schematic diagram.
Fig. 3 is adopted metal lead wire Rockwell hardness schematic diagram.。
Fig. 4 is adopted welding curve synoptic diagram.
Fig. 5 is the metal lead wire and the alumina-ceramic bonding strength schematic diagram that adopt the present invention to prepare sample.
Embodiment
As shown in Figure 1, low-stress alumina-ceramic metal sealing method, comprises the steps:
1) prepare alumina-ceramic, its alumina content accounts for 92 ~ 95wt%, adopts the method for flow casting molding to be processed into 0.2 ~ 5mm and to improve people's living condition ceramics;
2) metallization pattern makes, and adopts screen mask version, and molybdenum, molybdenum-manganese or the tungsten metallization paste deposition that can realize burning altogether with alumina-ceramic by the mode of printing are on ceramics;
3) fervent, worktable is heated to 25 DEG C ~ 65 DEG C, cuts into single with blade by the ceramics containing multiple assembly, the single ceramics cutting into multiple assembly is sent in high temperature sintering furnace; ;
4) high temperature sintering, the single ceramics cutting into multiple assembly is sent in high temperature sintering furnace, high temperature sintering in-furnace temperature 1500 ~ 1650 DEG C, carry out under vacuum, hydrogen or nitrogen atmosphere, in sintering process, at alumina-ceramic base substrate, molybdenum, molybdenum-manganese or tungsten metallization layer, and there is chemistry or physical reaction between ceramic body and metal layer, form the glassy phase of melting respectively, when molybdenum, molybdenum-manganese or tungsten metallization layer mortise after temperature is reduced to room temperature are on the ripe base of pottery;
5) prepare middle layer plating solution, formula is as table 1:
Table 1 middle layer electroplate liquid formulation
| NiSO 4·6H 2O | 15～25g/L |
| NaH 2PO 2·H 2O | 4～10g/L |
| (CH 2COONa) 2·6H 2O | 10～20g/L |
| NaCl | 8～15g/L |
| Buffer reagent PNG | 5～8g/L |
| Auxiliary complex-former PGS | 1～5g/L |
| Stablizer | 1～1.5mg/L |
| pH | 3.5～5 |
6) plating, in order to deposit one deck nickel on alumina-ceramic molybdenum, molybdenum-manganese or tungsten metallization layer,
The method of nickel plating, comprises the steps:
1. OP clean metal porcelain piece 3 ~ 5min is used;
2. deionized water rinsing 1 ~ 2min;
3. caustic dip: by aqueous slkali soaking, control pH is 9 ~ 12, and the time is 1 ~ 8min, temperature 50 ~ 80 DEG C, takes out, ultrasonic with deionized water;
4. pickling: soak with acid solution, control pH is 2 ~ 4, temperature 40 ~ 90 DEG C, time 1 ~ 10min, takes out, deionized water rinsing;
5. enter nickel bath, the time is 8 ~ 40min, takes out, washes down, dry and test intermediate layer thickness as Fig. 2 with deionized water;
7) metal lead wire and solder sheet pre-treatment, its pretreatment process, comprises the steps:
1. use toluene, acetone or soaked in absolute ethyl alcohol, time 1 ~ 10min, take out and dry;
2. cleaned metal lead wire is put into retort furnace, pass into protective atmosphere nitrogen, be heated to 1100 ~ 1170 DEG C, insulation 30 ~ 200min furnace cooling, test metal lead wire Rockwell hardness is as Fig. 3;
8) soldering is shelved, metallization alumina-ceramic, solder sheet, metal lead wire are loaded in graphite mo(u)ld successively, press and add tamponade, put into hydrogen atmosphere and shelve soldering by the welding curve (as Fig. 4) of the chain type soldering oven of processing requirement setting heating-cooling speed, taking-up sample test metal lead wire and alumina-ceramic bonding strength are as Fig. 5.
Embodiment
First adopt the method for flow casting molding to be processed into 0.6mm thick, alumina content accounts for the ceramic chips of 95wt%; The tungsten metallization paste deposition that can realize burning altogether with alumina-ceramic by the mode of printing is on ceramics; Heating station to 65 DEG C, cuts into single with blade by the ceramics containing multiple assembly; Advance high temperature sintering furnace, in-furnace temperature 1500 ~ 1650 DEG C, hydrogen atmosphere, obtain the ripe porcelain of tungsten metallization aluminum oxide;
Secondly, according to table 2 component design preparation middle layer plating solution, on aluminum oxide ripe porcelain tungsten metallization layer, nickel dam is applied according to plating technic;
Table 2 middle layer nickel plating bath composition
| NiSO 4·6H 2O | 20g/L |
| NaH 2PO 2·H 2O | 8g/L |
| (CH 2COONa) 2·6H 2O | 15g/L |
| NaCl | 12g/L |
| Buffer reagent PNG | 6g/L |
| Auxiliary complex-former PGS | 2g/L |
| Stablizer | 1mg/L |
| pH | 4 |
Then, carry out cleaning and annealing according to metal lead wire and solder sheet pretreatment technology, obtain the metal lead wire of low Rockwell hardness;
Finally, metallization alumina-ceramic, solder sheet, metal lead wire are loaded in graphite mo(u)ld successively, presses and add tamponade, put into hydrogen atmosphere and by the chain type soldering oven of processing requirement setting heating-cooling speed.
Claims (9)
1. low-stress alumina-ceramic metal sealing method, is characterized in that comprising the steps:
1) alumina-ceramic is prepared;
2) metallization pattern makes;
3) fervent;
4) high temperature sintering;
5) middle layer plating solution is prepared;
6) plating;
7) metal lead wire and solder sheet pre-treatment;
8) soldering is shelved.
2. low-stress alumina-ceramic metal sealing method according to claim 1, it is characterized in that described step 1) prepares alumina-ceramic, its alumina content accounts for 92 ~ 95wt%, adopts the method for flow casting molding to be processed into 0.2 ~ 5mm and to improve people's living condition ceramics.
3. low-stress alumina-ceramic metal sealing method according to claim 1, it is characterized in that described step 2) metallization pattern making, adopt screen mask version, molybdenum, molybdenum-manganese or the tungsten metallization paste deposition that can realize burning altogether with alumina-ceramic by the mode of printing are on ceramics.
4. low-stress alumina-ceramic metal sealing method according to claim 1, it is characterized in that described step 3) is fervent, worktable is heated to 25 DEG C ~ 65 DEG C, cuts into single with blade by the ceramics containing multiple assembly, the single ceramics cutting into multiple assembly is sent in high temperature sintering furnace.
5. low-stress alumina-ceramic metal sealing method according to claim 1, it is characterized in that described step 4) high temperature sintering, the single ceramics cutting into multiple assembly is sent in high temperature sintering furnace, high temperature sintering in-furnace temperature 1500 ~ 1650 DEG C, vacuum, carry out under hydrogen or nitrogen atmosphere, in sintering process, at alumina-ceramic base substrate, molybdenum, molybdenum-manganese or tungsten metallization layer, and there is chemistry or physical reaction between ceramic body and metal layer, form the glassy phase of melting respectively, molybdenum after temperature is reduced to room temperature, molybdenum-manganese or tungsten metallization layer mortise are on the ripe base of pottery.
6. low-stress alumina-ceramic metal sealing method according to claim 1, is characterized in that described step 5) preparation middle layer plating solution, its composition proportion:
。
7. low-stress alumina-ceramic metal sealing method according to claim 1, it is characterized in that described step 6) plating, the method for nickel plating, comprises the steps:
1. OP clean metal porcelain piece 3 ~ 5min is used;
2. deionized water rinsing 1 ~ 2min;
3. caustic dip: by aqueous slkali soaking, control pH is 9 ~ 12, and the time is 1 ~ 8min, temperature 50 ~ 80 DEG C, takes out, ultrasonic with deionized water;
4. pickling: soak with acid solution, control pH is 2 ~ 4, temperature 40 ~ 90 DEG C, time 1 ~ 10min, takes out, deionized water rinsing;
5. enter nickel bath, the time is 8 ~ 40min, takes out, washes down, dry and test intermediate layer thickness with deionized water.
8. low-stress alumina-ceramic metal sealing method according to claim 1, it is characterized in that described step 7) metal lead wire and solder sheet pre-treatment, its pretreatment process, comprises the steps:
1. use toluene, acetone or soaked in absolute ethyl alcohol, time 1 ~ 10min, take out and dry;
2. cleaned metal lead wire is put into retort furnace, pass into protective atmosphere nitrogen, be heated to 1100 ~ 1170 DEG C, insulation 30 ~ 200min furnace cooling, test metal lead wire Rockwell hardness.
9. low-stress alumina-ceramic metal sealing method according to claim 1, it is characterized in that described step 8) shelves soldering, metallization alumina-ceramic, solder sheet, metal lead wire are loaded in graphite mo(u)ld successively, press and add tamponade, put into hydrogen atmosphere and shelve soldering by the chain type soldering oven of processing requirement setting heating-cooling speed, taking out sample test metal lead wire and alumina-ceramic bonding strength.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114951880A (en) * | 2022-06-13 | 2022-08-30 | 宁波江丰电子材料股份有限公司 | Method for welding three-layer structure ceramic target |
Citations (3)
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|---|---|---|---|---|
| CN102400195A (en) * | 2011-11-23 | 2012-04-04 | 安徽华东光电技术研究所 | Nickel plating method after metallization of aluminum oxide ceramic |
| CN102795894A (en) * | 2012-08-09 | 2012-11-28 | 浙江亚通金属陶瓷有限公司 | Surface metallization layer of high-purity alumina ceramics and compounding technology thereof |
| CN104058733A (en) * | 2014-07-04 | 2014-09-24 | 娄底市安地亚斯电子陶瓷有限公司 | Vacuum-sealed high-capacity direct-current relay ceramic shell and manufacturing method thereof |
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- 2015-12-01 CN CN201510865925.7A patent/CN105481414B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400195A (en) * | 2011-11-23 | 2012-04-04 | 安徽华东光电技术研究所 | Nickel plating method after metallization of aluminum oxide ceramic |
| CN102795894A (en) * | 2012-08-09 | 2012-11-28 | 浙江亚通金属陶瓷有限公司 | Surface metallization layer of high-purity alumina ceramics and compounding technology thereof |
| CN104058733A (en) * | 2014-07-04 | 2014-09-24 | 娄底市安地亚斯电子陶瓷有限公司 | Vacuum-sealed high-capacity direct-current relay ceramic shell and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 蒋文娟等: "钨金属化氧化铝陶瓷基片的脱脂工艺研究", 《硅酸盐通报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114951880A (en) * | 2022-06-13 | 2022-08-30 | 宁波江丰电子材料股份有限公司 | Method for welding three-layer structure ceramic target |
| CN114951880B (en) * | 2022-06-13 | 2024-05-14 | 宁波江丰电子材料股份有限公司 | Method for welding three-layer ceramic target |
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