CN107382284A - A kind of sintering method of high temperature co-firing aluminium oxide ceramics - Google Patents
A kind of sintering method of high temperature co-firing aluminium oxide ceramics Download PDFInfo
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- CN107382284A CN107382284A CN201710505469.4A CN201710505469A CN107382284A CN 107382284 A CN107382284 A CN 107382284A CN 201710505469 A CN201710505469 A CN 201710505469A CN 107382284 A CN107382284 A CN 107382284A
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- aluminum oxide
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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
- 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
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
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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
- 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
- C04B35/64—Burning or sintering processes
- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/404—Refractory metals
Abstract
The present invention is a kind of sintering method of high temperature co-firing aluminium oxide ceramics, and this method comprises the following steps：（1）Using aluminum oxide green and Metal slurry aluminum oxide green part is made according to multi-layer ceramics production technology；（2）Aluminum oxide green part is placed on to hold and burnt in device；（3）The aluminum oxide green part dumping burnt in device will be held；（4）The aluminum oxide green part that will be held after dumping in burning device sinters in sintering furnace.Advantages of the present invention：1）This method can prepare high temperature co-firing aluminium oxide ceramics, applied to highly reliable, airtight device encapsulation and multi-chip module（MCM）The field such as substrate and shell.2）Sintered using the method for the present invention, the density of obtained common burning aluminium oxide ceramics is more than 3.60g/cm3, rupture strength be more than 300MPa, 1mm2The stretching resistance of metallization area is more than 20N, and performance meets the requirement of electronic ceramics.
Description
Technical field
The present invention relates to a kind of high temperature co-firing aluminum oxide（Al2O3）The sintering method of ceramics, belongs to electronic ceramics technology
Field, it is mainly used in highly reliable, airtight device encapsulation and multi-chip module（MCM）The field such as substrate and shell.
Background technology
HTCC（HTCC）The most frequently used material system is aluminium oxide ceramics system.Alumina high temperature common burning porcelain
Major advantage be insulate, high mechanical strength, corrosion-resistant and high frequency characteristics are good etc., be mainly used in highly reliable, airtight device
The field such as encapsulation and MCM substrates and shell.Alumina Ceramics Sintering temperature is higher, typically at 1500 DEG C~1650 DEG C, therefore with
Common burning metal paste must high temperature resistant, it is general to be used as the Metal slurry that aluminum oxide burns altogether using tungsten.
The high temperature co-firing of aluminum oxide is sintered due to there is metallization tungsten, it is necessary to is sintered under reducing atmosphere, is prevented metal height
Temperature aoxidizes, and the common burning of aluminum oxide also needs to certain oxidizing atmosphere and realizes ceramics and the common burning of metallization in addition, typically burns altogether
Atmosphere is controlled in certain dew point using the reducing atmosphere humidified.The sintering temperature of pure alumina is very high, it is difficult to real
Now burn altogether.A small amount of sintering aid is typically added in aluminum oxide to reduce the sintering temperature of ceramics, while realizes ceramics and gold
The good combination of categoryization.The making of high temperature co-firing aluminium oxide ceramics green ceramic part is typically using casting technique production green band, green
Band reuses green processing technology and makes green part.Green part contains a certain amount of binding agent, plasticizer and a small amount of solvent, to protect
The quality of card sintering porcelain piece must be clean by these organic matter removals before sintering, and here it is binder removal.Binder removal can be with
Carry out, can also be completed in sintering furnace in single draft glue discharging furnace, the high temperature co-firing technique typically produced in batches uses high temperature
Atmosphere push pedal sintering furnace carries out the dumping and sintering of green part.High temperature co-firing, which is held, burns breathing freely when device must simultaneously meet dumping
Property to ensure the abundant of dumping, and can ensure during high temperature sintering load bearing board it is smooth it is indeformable, device is firm is not prone to tip over, be high temperature
A key device of Alumina Ceramics Sintering is burnt altogether.
The content of the invention
Proposed by the present invention is a kind of sintering method of high temperature co-firing aluminium oxide ceramics, and its object is to using rational high
Temperature burns Alumina Ceramics Sintering device altogether, and porcelain piece when ensureing abundant volatilization and the sintering of organic matter during dumping is smooth and steady
It is fixed, so that the aluminum oxide common burning porcelain consistency, rupture strength and the Metallization strength that sinter out meet ceramic substrate, encapsulation
The requirement of shell etc..
The technical solution of the present invention：A kind of sintering method of high temperature co-firing aluminium oxide ceramics, comprises the following steps：
（1）Using aluminum oxide green and Metal slurry aluminum oxide green part is made according to multi-layer ceramics production technology；
（2）Aluminum oxide green part is placed on to hold and burnt in device；
（3）The aluminum oxide green part dumping burnt in device will be held；
（4）The aluminum oxide green part that will be held after dumping in burning device sinters in high-temperature atmosphere sintering furnace.
Advantages of the present invention：
1）This method can prepare high temperature co-firing aluminium oxide ceramics, applied to highly reliable, airtight device encapsulation and multi-chip module
（MCM）The field such as substrate and shell；
2）Sintered using the method for the present invention, it is ensured that green part dumping is fully and sintering porcelain piece flatness is good, and what is obtained is total to
Consistency, rupture strength and the Metallization strength for burning aluminium oxide ceramics meet the requirement of electronic ceramics.
Brief description of the drawings
Fig. 1 is that this sintering method holds burning device charging process schematic diagram.
Fig. 2-a and Fig. 2-b are the structural representations of this sintering method load bearing board, and wherein Fig. 2-a are load bearing board structure main views
Figure, Fig. 2-b are Fig. 2-a A-A profiles.
Fig. 3-a and Fig. 3-b are that this sintering method holds the structural representation for burning pillar, and wherein Fig. 3-a are to hold burning corbeling
Front view, Fig. 3-b are Fig. 3-a B-B profiles.
Fig. 4 is to hold burning device structure schematic diagram after this sintering method feeds.
Embodiment
A kind of sintering method of high temperature co-firing aluminium oxide ceramics, comprises the following steps：
（1）Using aluminum oxide green and Metal slurry aluminum oxide green part is made according to multi-layer ceramics production technology；
（2）Aluminum oxide green part is placed on to hold and burnt in device；
（3）The aluminum oxide green part dumping burnt in device will be held；
（4）The aluminum oxide green part that will be held after dumping in burning device sinters in sintering furnace.
The multi-layer ceramics production technology comprises the steps of：It is cast ceramic chips, ceramic chips printed metallization slurry, green
Piece lamination layer swaging is into multilayer ceramics, laminated ceramic chips earnestly into green part.
Described aluminum oxide green component includes Al2O3Powder, sintering aid, binding agent and plasticizer, wherein Al2O3The weight of powder
Amount accounts for the 80% ~ 85% of gross weight, and the weight of sintering aid accounts for the 3% ~ 6% of gross weight, and the weight of binding agent accounts for the 3% ~ 6% of gross weight,
The weight of solvent accounts for the 9% ~ 15% of gross weight.
Described Metal slurry composition includes tungsten powder, ceramic powder, binding agent and solvent, and the weight of wherein tungsten powder accounts for gross weight
The 85% ~ 90% of amount, the weight of ceramic powder accounts for the 2% ~ 5% of gross weight, and the weight of binding agent accounts for the 2% ~ 5% of gross weight, the weight of solvent
Amount accounts for the 5% ~ 10% of gross weight.
Described be placed on aluminum oxide green part is held in burning device, and specific method is as follows：
1）Green part is placed on load bearing board, load bearing board uses molybdenum plate, has circular hole on molybdenum plate；
2）Load bearing board pillar is placed in the circular hole on load bearing board, load bearing board pillar is cylindrical molybdenum post, and upper and lower surface, which has, to be stretched
The small column gone out, it is embedded in the circular hole of load bearing board；
3）By multilayer load bearing board, aluminum oxide green part product and hold and burn the pillar composition that is stacked together and hold burning device.
It is described to hold the aluminum oxide green part dumping burnt in device：Dumping atmosphere is the reducing atmosphere of nitrogen or humidification,
Dumping heating rate is less than 5 DEG C/min, 350 DEG C~600 DEG C of maximum temperature.
It is described to be sintered mounted in the aluminum oxide green part held in burning device in high-temperature atmosphere sintering furnace：Sintering atmosphere is to add
Wet reducing atmosphere, 1500 DEG C~1650 DEG C of sintered heat insulating temperature, soaking time 0.5~3 hour.
By the present invention in that with reasonably burning device is held, the abundant dumping of organic matter in green part can be caused, and keep burning
Green part is smooth and firm during knot, ensures to burn consistency, rupture strength and the Metallization strength of aluminium oxide ceramics altogether.Use this
The density of the high temperature co-firing aluminium oxide ceramics of method sintering is more than 3.60g/cm3, ceramic rupture strength is more than 300MPa, golden
Categoryization bonding area 1mm2Bear pulling force and be more than 20N；The high temperature multilayer co-firing aluminium oxide ceramics of this method sintering can be applied to height
Reliably, airtight device encapsulation and multi-chip module（MCM）The field such as substrate and shell.
With reference to embodiment, the invention will be further described.
Embodiment 1
Prepare the sintering method of high temperature co-firing aluminium oxide ceramics, wherein dumping uses single draft glue discharging furnace, and this method is as follows：
1）Take the Al for accounting for gross weight 85%2O3Powder, 6% sintering aid, 6% binding agent, 3% plasticizer, and additionally add 10%
Solvent configures green slurry, and Al is produced by casting technique2O3Ceramic chips；
2）Take the tungsten powder for accounting for gross weight 90%, 5% binding agent, 5% solvent configuration tungsten Metal slurry；
3）Ceramic chips surface tungsten Metal slurry is printed by printing screen technique；
4）Some ceramic chips are formed multi-layer green ceramic part, while separately take some ceramic chips to pass through lamination, heat by lamination, hot pressing
Pressure, raw cutting process make the green standard specimen of rupture strength and density measurement；
5）Green part and green standard specimen are loaded in the way of accompanying drawing 1 and hold burning device；
6）Burning device will be held equipped with green part, be put into dumping in draft glue discharging furnace.Dumping atmosphere is nitrogen, nitrogen flow 3m3/h。
Dumping heating rate is 1 DEG C/min, and 450 DEG C of dumping holding temperature, soaking time 3 hours, less than 450 DEG C cool with stove；
7）The burning device that holds that green part is housed after dumping is put into high-temperature atmosphere sintering furnace.High temperature sintering furnace heating rate is set
10 DEG C/min, 1600 DEG C of holding temperature are set to, atmosphere is set as 1 using the hydrogen and nitrogen mixed gas humidified, soaking time
Hour.Rate of temperature fall is 5 DEG C/min, and less than 500 DEG C cool with stove；
8）By the aluminium oxide ceramics sintered and test standard specimen taking-up is tested and performance test.
Using the rupture strength of rupture strength standard specimen test ceramics, the close of aluminium oxide ceramics is tested using density measurement standard specimen
Degree, is 1mm in metallization area2Metallization pattern on by first nickel plating, then with silver-copper brazing alloy welding can cut down the mode of lead
Measurement metallization and the bond strength of aluminium oxide ceramics.
The test result of the aluminium oxide ceramics rupture strength sintered using this method is shown in Table 1, ceramic thermal conductivity test knot
Fruit is shown in Table 2, and the extension weight pulling force of 5 metallized samples of test is all greater than 20N.
The aluminium oxide ceramics rupture strength test data of table 1
The aluminium oxide ceramics thermal conductivity test data of table 2
。
Embodiment 2
The sintering method of high temperature co-firing aluminium oxide ceramics is prepared, wherein dumping and sintering all enters in high-temperature atmosphere push pedal sintering furnace
OK, this method is as follows：
1）Make green part and load and hold burning device, its method is the same as embodiment 1；
2）High-temperature atmosphere push pedal sintering furnace technological parameter is set, and wherein maximum temperature sets 1600 DEG C, wherein the dumping section highest temperature
Spend for 500 DEG C, total 26 hours cycles of operation, atmosphere is the nitrogen and hydrogen gas mixture of humidification, and total gas couette is 10 m3/
h；
3）By equipped with green part holding burn device erection sequence be successively placed in the push pedal of sintering furnace, sintering furnace automatically by product according to
In secondary push-in sintering furnace, dumping section dumping is first passed through, heating is then proceeded to and is sintered into high temperature sintering section.
Held after the completion of sintering and burn device and porcelain piece and come out of the stove successively with push pedal, porcelain piece is removed from holding to burn in device, examined
Test and test.
Claims (7)
- A kind of 1. sintering method of high temperature co-firing aluminium oxide ceramics, it is characterized in that comprising the following steps：（1）Using aluminum oxide green and Metal slurry aluminum oxide green part is made according to multi-layer ceramics production technology；（2）Aluminum oxide green part is placed on to hold and burnt in device；（3）The aluminum oxide green part dumping burnt in device will be held；（4）The aluminum oxide green part that will be held after dumping in burning device sinters in sintering furnace.
- 2. the sintering method of high temperature co-firing aluminium oxide ceramics according to claim 1, it is characterized in that the multi-layer ceramics produces Technique comprises the steps of：Be cast ceramic chips, ceramic chips printed metallization slurry, ceramic chips lamination layer swaging into multilayer ceramics, Laminated ceramic chips are earnestly into green part.
- 3. the sintering method of high temperature co-firing aluminium oxide ceramics according to claim 1, it is characterized in that described aluminum oxide green Component includes Al2O3Powder, sintering aid, binding agent and plasticizer, wherein Al2O3The weight of powder accounts for the 80% ~ 85% of gross weight, helps burning The weight of agent accounts for the 3% ~ 6% of gross weight, and the weight of binding agent accounts for the 3% ~ 6% of gross weight, the weight of solvent account for gross weight 9% ~ 15%。
- 4. the sintering method of high temperature co-firing aluminium oxide ceramics according to claim 1, it is characterized in that described Metal slurry Composition includes tungsten powder, ceramic powder, binding agent and solvent, and the weight of wherein tungsten powder accounts for the 85% ~ 90% of gross weight, the weight of ceramic powder The 2% ~ 5% of gross weight is accounted for, the weight of binding agent accounts for the 2% ~ 5% of gross weight, and the weight of solvent accounts for the 5% ~ 10% of gross weight.
- 5. the sintering method of high temperature co-firing aluminium oxide ceramics according to claim 1, it is characterized in that described give birth to aluminum oxide Porcelain piece, which is placed on to hold, burns in device, and specific method is as follows：1）Green part is placed on load bearing board, load bearing board uses molybdenum plate, has circular hole on molybdenum plate；2）Load bearing board pillar is placed in the circular hole on load bearing board, load bearing board pillar is cylindrical molybdenum post, and upper and lower surface, which has, to be stretched The small column gone out, it is embedded in the circular hole of load bearing board；3）By multilayer load bearing board, aluminum oxide green part product and hold and burn the pillar composition that is stacked together and hold burning device.
- 6. the sintering method of high temperature co-firing aluminium oxide ceramics according to claim 1, it is characterized in that described will hold is burnt in device Aluminum oxide green part dumping：Dumping atmosphere is the reducing atmosphere of nitrogen or humidification, and dumping heating rate is less than 5 DEG C/min, 350 DEG C~600 DEG C of maximum temperature.
- 7. the sintering method of high temperature co-firing aluminium oxide ceramics according to claim 1, it is characterized in that described will be mounted in holds burning dress The aluminum oxide green part put sinters in high-temperature atmosphere sintering furnace：Sintering atmosphere be humidification reducing atmosphere, sintered heat insulating 1500 DEG C~1650 DEG C of temperature, soaking time 0.5~3 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053196A (en) * | 2018-07-12 | 2018-12-21 | 中国电子科技集团公司第五十五研究所 | A kind of sintering method of large scale high-temperature co-fired ceramics |
| CN110632338A (en) * | 2019-11-12 | 2019-12-31 | 中国电子科技集团公司第四十九研究所 | Sensitivity probe with co-firing structure for eddy current type high-temperature rotating speed sensor and preparation method thereof |
| CN111365985A (en) * | 2019-12-26 | 2020-07-03 | 横店集团东磁股份有限公司 | Hydrogen-protected molybdenum wire push plate sintering furnace |
| CN112496319A (en) * | 2019-09-16 | 2021-03-16 | 宿迁启祥电子科技有限公司 | Sintering device and preparation method of tungsten alloy material |
| CN114502325A (en) * | 2019-10-19 | 2022-05-13 | 株式会社村田制作所 | Clip for chip electronic component |
| CN114804837A (en) * | 2022-03-14 | 2022-07-29 | 中国电子科技集团公司第四十三研究所 | Multilayer tungsten metalized alumina special-shaped piece for HTCC and preparation method thereof |
| CN115259869A (en) * | 2022-07-29 | 2022-11-01 | 苏州瑞瓷新材料科技有限公司 | Firing-bearing raw porcelain and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053196A (en) * | 2018-07-12 | 2018-12-21 | 中国电子科技集团公司第五十五研究所 | A kind of sintering method of large scale high-temperature co-fired ceramics |
| CN109053196B (en) * | 2018-07-12 | 2021-01-26 | 中国电子科技集团公司第五十五研究所 | Sintering method of large-size high-temperature co-fired ceramic |
| CN112496319A (en) * | 2019-09-16 | 2021-03-16 | 宿迁启祥电子科技有限公司 | Sintering device and preparation method of tungsten alloy material |
| CN114502325A (en) * | 2019-10-19 | 2022-05-13 | 株式会社村田制作所 | Clip for chip electronic component |
| CN110632338A (en) * | 2019-11-12 | 2019-12-31 | 中国电子科技集团公司第四十九研究所 | Sensitivity probe with co-firing structure for eddy current type high-temperature rotating speed sensor and preparation method thereof |
| CN111365985A (en) * | 2019-12-26 | 2020-07-03 | 横店集团东磁股份有限公司 | Hydrogen-protected molybdenum wire push plate sintering furnace |
| CN114804837A (en) * | 2022-03-14 | 2022-07-29 | 中国电子科技集团公司第四十三研究所 | Multilayer tungsten metalized alumina special-shaped piece for HTCC and preparation method thereof |
| CN115259869A (en) * | 2022-07-29 | 2022-11-01 | 苏州瑞瓷新材料科技有限公司 | Firing-bearing raw porcelain and preparation method and application thereof |
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