KR101417445B1 - MgO substrate compounds for middle temperature co-fired ceramics - Google Patents
MgO substrate compounds for middle temperature co-fired ceramics Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- 239000000758 substrate Substances 0.000 title abstract description 30
- 150000001875 compounds Chemical class 0.000 title 1
- 239000011521 glass Substances 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 24
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 8
- 229910052810 boron oxide Inorganic materials 0.000 claims description 6
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims description 4
- 239000005297 pyrex Substances 0.000 claims description 4
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 89
- 239000000395 magnesium oxide Substances 0.000 abstract description 38
- 238000010344 co-firing Methods 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 24
- 239000003513 alkali Substances 0.000 description 8
- 238000010304 firing Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007088 Archimedes method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 210000001672 ovary Anatomy 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/82—Asbestos; Glass; Fused silica
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B35/01—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
- C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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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
- C04B35/64—Burning or sintering processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
본 발명은 적층 세라믹 기판을 제조함에 있어 가격이 저렴한 Ni 전극과 동시소성이 가능하도록 1400 ℃이하에서 소결특성과 Ni 전극과의 접합성이 우수한 마그네시아 세라믹 기판 조성물을 제공하는 것이다. 이를 위하여 본 발명은 Ni 전극과 열팽창계수가 비슷하고 열전도도가 높은 마그네시아(MgO)에 소결조제로 양질의 유리분말(glass powder) 또는 산화붕소(B2O3)나 산화바나듐(V2O5)를 적당량 첨가함으로써 소결특성을 개선시킨 마그네시아 세라믹 기판 조성물에 관한 것이다. An object of the present invention is to provide a magnesia ceramic substrate composition excellent in sintering property and bonding property to a Ni electrode at a temperature of 1400 ° C or lower so as to be capable of co-firing with a Ni electrode which is inexpensive in manufacturing a multilayer ceramic substrate. For this purpose, the present invention relates to a method for producing a sintered body by adding an appropriate amount of high quality glass powder, boron oxide (B2O3) or vanadium oxide (V2O5) to magnesia (MgO) having thermal expansion coefficient similar to that of a Ni electrode and having high thermal conductivity, To a magnesia ceramic substrate composition having improved properties.
Description
본 발명은 적층세라믹 기판을 제조함에 있어 가격이 저렴한 Ni 전극과 동시소성이 가능하도록 1400 ℃이하에서 소결특성과 Ni 전극과의 접합성이 우수한 마그네시아 세라믹 기판 조성물을 제공하는 것이다. 이를 위하여 본 발명은 Ni 전극과 열팽창계수가 비슷하고 열전도도가 높은 마그네시아(MgO)에 소결조제로 양질의 유리분말(glass powder) 또는 산화붕소(B2O3)나 산화바나듐(V2O5)를 적당량 첨가함으로써 소결특성을 개선시킨 마그네시아 세라믹 기판 조성물에 관한 것이다.
An object of the present invention is to provide a magnesia ceramic substrate composition excellent in sintering property and bonding property to a Ni electrode at a temperature of 1400 ° C or lower so as to be capable of co-firing with a Ni electrode which is inexpensive in manufacturing a multilayer ceramic substrate. For this purpose, the present invention relates to a method for producing a sintered body by adding an appropriate amount of high quality glass powder, boron oxide (B2O3) or vanadium oxide (V2O5) to magnesia (MgO) having thermal expansion coefficient similar to that of a Ni electrode and having high thermal conductivity, To a magnesia ceramic substrate composition having improved properties.
일반적으로 세라믹은 선행기술인 등록특허 10-0326874호 등에서 제시되는 바와 같이, 히터용으로 주로 사용되고 있고, 주로 고온소성(1500 ∼ 1600 ℃)에서 소성이 이루어진다. Generally, ceramics are mainly used for heaters as shown in the prior art Patent No. 10-0326874, and they are mainly fired at high temperature (1500 to 1600 ° C).
근래 세라믹 기판은 전자회로 기판, LED 방열기판등에 주로 사용되며, 최근 전자회로의 집적도가 증가하면서 배선의 고밀도와 다층 집적화로 급속히 변화하고 있어 전극과 동시소성이 가능한 적층세라믹 기판용 소재가 크게 요구되고 있다.
In recent years, ceramics substrates are mainly used for electronic circuit boards, LED radiator boards, etc. Recently, as the degree of integration of electronic circuits has increased, materials for multilayer ceramic substrates that can be co- have.
적층세라믹 기판소재는 사용전극과 (1)우수한 동시소결 특성, (2)유사한 열팽창계수, (3) 내구성을 위한 적당한 휨강도, (4)전극과의 우수한 접합성, (5)저가격이 요구되며, 현재, 표1에서와 같이 고온소성(1500 ∼ 1600 ℃)용으로 알루미나(Al2O3) 로 조성된 기판재료와 저온소성(850 ∼ 925℃)용으로는 유리/세라믹 복합재료가 주로 사용되고 있다.
The multilayer ceramic substrate material is required to have (1) excellent co-sintering characteristics, (2) similar thermal expansion coefficient, (3) adequate bending strength for durability, (4) As shown in Table 1, substrate materials composed of alumina (Al2O3) for high temperature firing (1500 ~ 1600 ℃) and glass / ceramics composites for low temperature firing (850 ~ 925 ℃) are mainly used.
그러나, 고온 동시 소성는 소결성, 기계적 강도, 전극 접합성 및 열전도성 면에서는 우수하나 고가의 전극과 높은 소성온도로 인한 생산수율과 단가가 큰 문제이며, 유리/세라믹의 경우는 다량 함유된 유리로 인해 소재의 가격이 높고 여러가지 특성들도 만족스럽지 못하다.
However, the high-temperature co-firing is excellent in terms of sintering property, mechanical strength, electrode bonding property and thermal conductivity, but the production yield and the unit cost are high due to expensive electrodes and high firing temperature. In case of glass / ceramics, The price is high and various characteristics are not satisfactory.
이러한 특성의 개선을 목적으로 많은 연구가 진행되고 있으나 부분적인 개선이 이루어질 뿐이며, 근본적인 해결방안이 도출되지 못하는 실정으로 적층세라믹 기판이 고집적화하는 추세속에 신뢰성을 확보하고 효율적인 생산을 위해서는 상기에서 설명한 요구조건을 만족할 수 있는 새로운 형태의 중온 동시소성용 세라믹 기판 조성물의 개발이 절실히 요구되고 있다. Although many studies have been conducted for the purpose of improving these characteristics, only a partial improvement is made and a fundamental solution can not be derived. In order to ensure reliability in a trend of high integration of a multilayer ceramic substrate and to produce efficiently, It is urgently required to develop a new type ceramic substrate composition for co-firing at mid-temperature.
[특허문헌][Patent Literature]
국내 등록특허 10-0326874호
Korean Patent No. 10-0326874
본 발명은 저가이고 전기 전도성이 양호한 Ni전극과 열팽창계수가 비슷하고 열전도도가 높은 마그네시아(MgO)에 소결조제로 양질의 유리분말(glass powder) 또는 산화붕소(B2O3)나 산화바나듐(V2O5)를 적당량 첨가함으로써 소결특성을 개선시킨 중온 동시소성용 마그네시아 세라믹 기판 조성물에 대한 연구를 거듭한 결과, 본 발명에 이르렀다.
The present invention relates to a method for producing a high-quality glass powder, boron oxide (B2O3), or vanadium oxide (V2O5) as a sintering aid in magnesia (MgO) having a thermal expansion coefficient similar to that of a Ni electrode having a low thermal conductivity and a high thermal conductivity, As a result of further studies on a magnesia ceramic substrate composition for co-firing at a middle temperature which is improved in sintering characteristics by adding an appropriate amount, the present invention has been accomplished.
본 발명의 목적은 적층 세라믹 기판을 제조함에 있어 가격이 저렴한 Ni 전극과 동시소성이 가능하도록 1400 ℃이하에서 소결특성과 Ni 전극과의 접합성이 우수한 중온 동시소성용 마그네시아 세라믹 기판 조성물을 제공하는 것이다.
An object of the present invention is to provide a magnesia ceramic substrate composition for middle-temperature co-firing having excellent sintering characteristics and bonding properties to a Ni electrode at 1400 ° C or lower so that co-firing can be performed with a Ni electrode having a low cost in producing a multilayer ceramic substrate.
본 발명은 Ni 전극과 열팽창계수가 비슷하고 열전도도가 높은 마그네시아(MgO)에 소결조제로 양질의 유리분말(glass powder) 또는 산화붕소(B2O3)나 산화바나듐(V2O5)를 적당량 첨가함으로써 소결특성을 개선시킨 마그네시아 세라믹 기판 조성물을 제공하고자 하는 것이다.The present invention relates to a method for producing a sintered powder by adding an appropriate amount of high quality glass powder, boron oxide (B2O3) or vanadium oxide (V2O5) to magnesia (MgO) having thermal expansion coefficient similar to that of a Ni electrode and having high thermal conductivity, And to provide an improved magnesia ceramic substrate composition.
본 발명에 의한 중온 동시소성용 마그네시아 세라믹 기판 조성물은 적층 세라믹 기판을 제조함에 있어 가격이 저렴한 Ni 전극과 동시소성이 가능하도록 1400 ℃이하에서 소결특성과 Ni 전극과의 접합성이 우수하고 양호한 열전도도를 부여함으로서, 적층세라믹 기판의 생산원가와 신뢰성을 크게 향상시켜 적용분야를 대폭 확대할 것으로 기대한다.
The magnesia ceramic substrate composition for co-firing at mid-temperature according to the present invention has excellent sintering property and bonding property to Ni electrode at 1400 ° C or less and good thermal conductivity so as to be co-fired with a low-cost Ni electrode in producing a multilayer ceramic substrate It is expected that the production cost and reliability of the multilayer ceramic substrate will be greatly improved and the application field will be greatly expanded.
도 1은 마그네시아에 유리분말을 첨가함에 따른 선수축율의 변화를 나타내는 그래프.
도 2는 마그네시아에 소결조제을 첨가함에 따른 선수축율의 변화를 나타내는 그래프.BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a graph showing the change in the linear shrinkage ratio when glass powder is added to magnesia. FIG.
FIG. 2 is a graph showing the change in the linear shrinkage ratio when the sintering aid is added to the magnesia.
본 발명은 저가이고 전기 전도성이 양호한 Ni전극과 열팽창계수가 비슷하고 열전도도가 높은 마그네시아(MgO)에 소결조제로 양질의 유리분말(glass powder) 또는 산화붕소(B2O3)나 산화바나듐(V2O5)등을 소결조제로 적당량 첨가함으로써 소결특성을 개선시킨 중온 동시소성용 마그네시아 세라믹 기판 조성물에 관한 것이다.
The present invention relates to a method for producing a high-quality glass powder, boron oxide (B2O3), vanadium oxide (V2O5), and the like, as a sintering auxiliary agent, on magnesia (MgO) having a thermal expansion coefficient similar to that of a Ni electrode having a low cost and good electrical conductivity, To a manganese ceramics substrate composition for co-firing at a middle temperature in which an appropriate amount of the sintering aid is added to improve sintering characteristics.
본 발명에 의한 1400 ℃이하에서 소결특성과 Ni 전극과의 접합성이 우수한 마그네시아 세라믹 기판 조성물의 조성비를 구체적으로 나타내면 다음과 같다.
The composition ratio of the magnesia ceramic substrate composition having the sintering property and the bonding property with the Ni electrode at 1400 ° C or lower according to the present invention will be described in detail as follows.
화학식 (100-x-y) MgO + x 유리분말 + y 소결조제 로 표시되는 식 중, x가 0 내지 30중량%이고, y는 0 내지 10중량% 이다.
X is from 0 to 30% by weight and y is from 0 to 10% by weight, expressed by the formula (100-xy) MgO + x glass powder + y sintering auxiliary.
본 발명의 중온 동시소성용 마그네시아 세라믹 기판 조성물은 저가이고 전기 전도성이 양호한 Ni전극과 동시소성을 위하여 우선, 열팽창계수가 비슷하고 열전도도가 산화물중 제일 높지만 소결이 어려운 마그네시아(MgO)의 소결온도를 1400 ℃이하로 낮추어야 한다. 이를 위해서는 저알카리 또는 무알카리 성분의 유리분말이나, 융점이 낮은 세라믹 분말을 소결조제로 적당량 첨가함으로서 Ni전극과 동시소성용 마그네시아 세라믹 기판 조성물의 제조가 가능하며, 이와 같은 본 발명의 조성물은 다음과 같은 일반적인 산화물 혼합 방법에 의해 용이하게 제조할 수 있다.
The magnesia ceramic substrate composition for co-firing at mid-temperature of the present invention has a low sintering temperature of magnesia (MgO) having a thermal expansion coefficient similar to that of the oxide but having the highest thermal conductivity but difficult to sinter for simultaneous firing with a Ni electrode having good electric conductivity It should be lowered to 1400 ℃ or lower. For this purpose, it is possible to prepare a magnesium-based ceramic substrate composition for co-firing with a Ni electrode by adding an appropriate amount of a low-alkali or non-alkaline glass powder or a low-melting-point ceramic powder with a sintering aid. Can be easily produced by a common oxide mixing method as described above.
먼저, 첨가제인 유리분말은 표2.에서 보는 바와같이 기판의 절연성을 높이고 소결중 변형을 방지하기 위하여 저알카리 또는 무알카리 성분의 유리를 사용하는 것이 바람직하며, 디스크 밀과 볼밀을 이용하여 잘 분쇄하여 2um정도의 입도가 되도록 제조한다.
As shown in Table 2, it is preferable to use low alkali or non-alkali glass in order to increase the insulating property of the substrate and prevent deformation during sintering. The glass powder is well pulverized using a disk mill and a ball mill 2 < / RTI > um.
중온 동시소성용 마그네시아 세라믹 기판을 위한 조성물은 표3.에서 보는 바와 같이 마그네시아(MgO)에 첨가제로 저알카리 또는 무알카리 성분의 유리분말이나, As shown in Table 3, the composition for a medium-temperature co-firing magnesia ceramic substrate is a glass powder of low alkali or non-alkali content as an additive to magnesia (MgO)
융점이 낮은 소결조제 분말을 적당량 첨가하여 볼밀에서 알코올을 용매로 혼합과 분쇄하여 건조시킨다. 건조된 혼합분말은 지름이 15mm안 원형의 금속몰드에서 100 MPa의 압력으로 성형한 후, 전기로를 이용하여 1250 ∼ 1400 ℃의 온도에서 2시간동안 소결한다.
An appropriate amount of sintering aid powder having a low melting point is added, and the alcohol is mixed and pulverized in a ball mill and dried. The dried mixed powder is molded at a pressure of 100 MPa in a metal mold having a circular inner diameter of 15 mm and then sintered in an electric furnace at a temperature of 1250 to 1400 ° C for 2 hours.
이렇게 제조된 소결체는 제조된 소결체는 선수축율과 아르키메데스법을 이용한 밀도측정을 통하여 소결특성을 평가하고, 조성물을 유기바인더 용액과 볼밀에서 혼합하여 500um두께로 테이프 성형 후 Ni전극을 인쇄하고 환원분위기 전기로를 이용하여 1350 ℃의 온도에서 2시간동안 소결하여 접합성을 평가하였다.
The sintered body thus manufactured was evaluated for sintering properties by measuring the linear shrinkage ratio and the density using the Archimedes method. The composition was mixed with an organic binder solution and a ball mill to form a tape with a thickness of 500 袖 m, then a Ni electrode was printed, And the sinterability was evaluated by sintering at 1350 ° C for 2 hours.
이하, 본 발명을 하기 실시예에 의해 더욱 상세히 설명하지만, 본 발명의 범위가 이들 실시예에만 국한되는 것은 아니다.
Hereinafter, the present invention will be described in more detail by way of the following examples, but the scope of the present invention is not limited to these examples.
<실시예>
<Examples>
중온 동시소성용 마그네시아 세라믹 기판을 위한 조성물은 표3.에서 보는 바와 같이 마그네시아(MgO)에 첨가제로 2um정도로 잘 분쇄시킨 저알카리 또는 무알카리 성분의 유리분말이나, 산화붕소(B2O3)나 산화바나듐(V2O5)과 같이 융점이 낮은 소결조제 분말을 적당량 첨가하여 볼밀에서 알코올을 용매로 혼합과 분쇄하여 건조시킨다. 건조된 혼합분말은 지름이 15mm안 원형의 금속몰드에서 100 MPa의 압력으로 성형한 후, 전기로를 이용하여 1250 ∼ 1400 ℃의 온도에서 2시간동안 소결한다.
As shown in Table 3, the composition for the co-fired magnesia ceramic substrate is a glass powder of a low-alkali or non-alkali content finely ground to about 2 μm as an additive to magnesia (MgO), or a glass powder of boron oxide (B2O3) V2O5) is added in an appropriate amount, and the alcohol is mixed and pulverized with a solvent in a ball mill and dried. The dried mixed powder is molded at a pressure of 100 MPa in a metal mold having a circular inner diameter of 15 mm and then sintered in an electric furnace at a temperature of 1250 to 1400 ° C for 2 hours.
이렇게 제조된 소결체는 제조된 소결체는 선수축율과 아르키메데스법을 이용한 밀도측정을 통하여 소결특성을 평가하고, 조성물을 유기바인더 용액과 볼밀에서 혼합하여 500um두께로 테이프 성형 후 Ni전극을 인쇄하고 환원분위기 전기로를 이용하여 1350 ℃의 온도에서 2시간동안 소결하여 접합성을 평가하였다.
The sintered body thus manufactured was evaluated for sintering properties by measuring the linear shrinkage ratio and the density using the Archimedes method. The composition was mixed with an organic binder solution and a ball mill to form a tape with a thickness of 500 袖 m, then a Ni electrode was printed, And the sinterability was evaluated by sintering at 1350 ° C for 2 hours.
실험 결과는 표3 와 도1, 도2에서 보는 바와 같다.
The experimental results are shown in Table 3 and FIGS. 1 and 2.
P glass: Pyrex glass, L glass: LCD glass
P glass: Pyrex glass, L glass: LCD glass
도1과 도2를 보면 난소결성인 마그네시아(MgO)가 적정량의 유리분말이나 소결조제가 첨가될 경우 선수축율의 차이는 있으나 1400℃ 이하에서도 소결수축이 충분히 이루어 짐을 알 수 있으며, 유리분말이나 소결조제의 첨가량이 증가 할수록 소결온도는 1250℃까지 점차 낮아짐을 볼 수 있다.
1 and 2 show that when an appropriate amount of glass powder or sintering additive is added to magnesia (MgO), which is an ovary, there is a difference in linear shrinkage but sintering shrinkage is sufficiently achieved even at 1400 ° C. or lower. The sintering temperature is gradually decreased to 1250 ℃ as the amount of the additive is increased.
따라서, Ni전극과 동시소성이 적합한 소결온도인 1250 ∼ 1350 ℃의 온도범위에서 마그네시아(MgO)에 적절한 첨가제와 첨가량을 알아보기 위해 표3에 나타낸 조성들에 대하여 실험한 결과, 첨가제의 첨가에 따른 마그네시아 세라믹 조성물의 소결특성들을 살펴보면, 1550 ℃에서도 치밀화되지 않는 마그네시아(MgO)가 유리분말이나 소결조제를 일정량이상 첨가할 경우 98%이상의 치밀한 세라믹스가 제조됨을 알 수 있다.
Therefore, in order to investigate the proper additives and the additive amount of magnesia (MgO) in the temperature range of 1250 ~ 1350 ° C, which is suitable for co-firing with the Ni electrode, the compositions shown in Table 3 were tested. The sintering characteristics of the magnesia ceramic composition are as follows: Magnesia (MgO) which is not densified even at 1550 ° C is produced with more than 98% of dense ceramics when a certain amount of glass powder or sintering aid is added.
이러한 결과를 바탕으로 유리분말의 경우 5 내지 30중량%, 그리고 소결조제 분말은 2 내지 10중량%가 바람직한 첨가량임을 확인하였다. 그러나, 이러한 경향은 첨가제의 첨가에 따른 액상생성에 의한 결과로, 기계적 강도나 열전도도등의 다른 특성의 저하요인이 될 수 있으므로 가급적 적은량의 첨가가 바람직하다.
Based on these results, it was confirmed that 5 to 30% by weight of the glass powder and 2 to 10% by weight of the sintering aid powder were preferable amounts. However, such a tendency may be a cause of deterioration of other properties such as mechanical strength and thermal conductivity as a result of liquid phase formation upon addition of an additive, so it is preferable to add a small amount as much as possible.
따라서, 유리 분말보다는 소결조제를 사용하는 경우 특성의 저하를 최소화하면서 치밀화가 가능하며, 소결조제인 산화바나듐(V2O5)과 산화붕소(B2O3)가 단독으로 첨가될 경우보다 서로 상호보완되어 적정량 첨가될때 더욱 우수한 특성이 발현됨을 알 수 있다.
Therefore, when using a sintering assistant rather than a glass powder, densification can be performed while minimizing the deterioration of characteristics. When the sintering assistant vanadium oxide (V2O5) and boron oxide (B2O3) are added to each other, And more excellent characteristics are exhibited.
한편, 본 발명에 따라 제조된 마그네시아(MgO) 테잎에 니켈(Ni)전극을 인쇄하여 1350 ℃의 온도에서 환원분위기에서 동시소성시킨 결과, 도3에서 보듯이 니켈(Ni)전극이 깨끗이 잘 접합되어 있음을 알 수 있다.
Meanwhile, a nickel (Ni) electrode was printed on the magnesia (MgO) tape manufactured according to the present invention and co-fired in a reducing atmosphere at a temperature of 1350 ° C. As a result, as shown in FIG. 3, .
본 발명에 의한 중온 동시소성용 마그네시아 세라믹 기판 조성물은 저가이고 전기 전도성이 양호한 Ni전극과 열팽창계수가 비슷하고 열전도도가 높은 마그네시아(MgO)에 소결조제로 양질의 유리분말(glass powder) 또는 산화붕소(B2O3)나 산화바나듐(V2O5) 등을 소결조제로 적당량 첨가함으로써 1400 ℃이하에서 소결특성과 Ni 전극과의 접합성이 우수한 특성을 갖는다. 이는 기존의 고온 동시소성(1500 ∼ 1600 ℃)용 기판소재인 알루미나(Al2O3)와 비교하여 낮은 소결온도와 저가 니켈전극을 사용하는 장점이 있으며, 기존의 저온소성(850 ∼ 925℃)용으로는 유리/세라믹 복합재료와 비교하면 가격과 특성이 우수하고 신뢰성 높은 중온 동시소성용 마그네시아 세라믹 기판 조성물을 제공한다.
The magnesia ceramic substrate composition for co-firing at mid-temperature according to the present invention is a low-cost and high-conductivity Ni electrode having a thermal expansion coefficient similar to that of magnesia (MgO) having high thermal conductivity. The sintering aid is a glass powder or a boron oxide (B2O3), vanadium oxide (V2O5), and the like are added in an appropriate amount as a sintering aid, and the sintering property and the bonding property to the Ni electrode are excellent at 1400 ° C or lower. It has advantages of low sintering temperature and low cost nickel electrode compared to alumina (Al2O3), which is a substrate material for high temperature co-firing (1500 ~ 1600 ℃), and it has advantages for low temperature firing (850 ~ 925 ℃) The present invention provides a magnesia ceramic substrate composition for co-firing at a middle temperature which is superior in price and characteristics and is more reliable than a glass / ceramic composite material.
Claims (3)
화학식 (100-x-y) MgO + x 유리분말 + y 소결조제 로 표시되는 식 중, x가 0 내지 30중량%이고, y는 0 내지 10중량%로 하되, 유리 분말은 파이렉스 유리 또는 LCD 전자기능성 유리를 분쇄하여 만든 첨가물이고, 소결조제의 분말은 산화바나듐을 단독 또는 산화붕소와 서로 혼합하여 만든 세라믹 첨가물임을 특징으로 하는 중온 동시소성용 마그네시아 세라믹 기판 조성물.
X is from 0 to 30% by weight and y is from 0 to 10% by weight, wherein the glass powder is at least one selected from the group consisting of Pyrex glass or LCD electronic functional glass And the powder of the sintering aid is a ceramic additive prepared by mixing vanadium oxide alone or with boron oxide. The composition of claim 1, wherein the sintering aid powder is a ceramic additive.
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