JPH0768065B2 - Glass-coated aluminum nitride sintered body and method for producing the same - Google Patents

Glass-coated aluminum nitride sintered body and method for producing the same

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Publication number
JPH0768065B2
JPH0768065B2 JP62234370A JP23437087A JPH0768065B2 JP H0768065 B2 JPH0768065 B2 JP H0768065B2 JP 62234370 A JP62234370 A JP 62234370A JP 23437087 A JP23437087 A JP 23437087A JP H0768065 B2 JPH0768065 B2 JP H0768065B2
Authority
JP
Japan
Prior art keywords
glass
sintered body
aluminum nitride
nitride sintered
heated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
JP62234370A
Other languages
Japanese (ja)
Other versions
JPS6479085A (en
Inventor
巌 平松
敏昭 坂井田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Electric Glass Co Ltd
Original Assignee
Nippon Electric Glass Co Ltd
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Filing date
Publication date
Application filed by Nippon Electric Glass Co Ltd filed Critical Nippon Electric Glass Co Ltd
Priority to JP62234370A priority Critical patent/JPH0768065B2/en
Publication of JPS6479085A publication Critical patent/JPS6479085A/en
Publication of JPH0768065B2 publication Critical patent/JPH0768065B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/12—Mountings, e.g. non-detachable insulating substrates
    • H01L23/14—Mountings, e.g. non-detachable insulating substrates characterised by the material or its electrical properties
    • H01L23/15—Ceramic or glass substrates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は表面を被覆したガラス層が熱膨張によって亀裂
を生ずることのないガラス被覆窒化アルミニウム焼結体
およびその製法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a glass-coated aluminum nitride sintered body in which a glass layer coated on the surface does not crack due to thermal expansion, and a method for producing the same.

〔従来の技術〕[Conventional technology]

窒化アルミニウム焼結体は、アルミナ焼結体のもつ電気
特性をほぼそのまま備えた焼結体で、半導体回路基板等
に用いられる高熱伝導性セラミックスとして広い用途が
見込まれている。The aluminum nitride sintered body is a sintered body that has almost the same electrical characteristics as the alumina sintered body, and is expected to find wide application as a high thermal conductive ceramic used in semiconductor circuit boards and the like.

しかし、窒化アルミニウム焼結体は水蒸気雰囲気中での
耐食性が低い。この対策として耐食性を高め、かつ表面
を平滑とするため、ガラス被覆を行なう方法が知られて
いる。However, the aluminum nitride sintered body has low corrosion resistance in a steam atmosphere. As a countermeasure against this, there is known a method of coating glass in order to enhance corrosion resistance and smooth the surface.

〔発明が解決しようとする問題点〕[Problems to be solved by the invention]

ところで、窒化アルミニウム焼結体を被覆するガラスと
しては、例えばPbO・SiO・Al2O3・ZrO系、BaO・SiO・B2
O3・TiO2系、PbO・SiO2・B2O3・Al2O3系、SiO2・Bi2O3
・B2O3・BaO系のように、アルミナ焼結体を被覆するの
に用いられるガラス組成物がそのまま使用されている
が、窒化アルミニウムよりも熱膨張係数が大きく、ガラ
ス被覆に亀裂を生ずる欠点があった。By the way, as the glass for coating the aluminum nitride sintered body, for example, PbO / SiO / Al 2 O 3 / ZrO system, BaO / SiO / B 2
O 3・ TiO 2 system, PbO ・ SiO 2・ B 2 O 3・ Al 2 O 3 system, SiO 2・ Bi 2 O 3
· B As 2 O 3 · BaO based, but glass composition used to coat the alumina sintered body is used as it is, a large thermal expansion coefficient than aluminum nitride, causing cracks in the glass coating There was a flaw.

本発明は上記の事情に鑑み、表面を被覆したガラス層に
気泡が残留せず、また亀裂をを発生することのないガラ
ス被覆窒化アルミニウム焼結体およびその製法を提供す
ることを目的とする。In view of the above circumstances, it is an object of the present invention to provide a glass-covered aluminum nitride sintered body in which bubbles do not remain in the surface-coated glass layer and cracks do not occur, and a method for producing the same.

〔問題点を解決するための手段〕[Means for solving problems]

本発明は上記の目的を達成すべくなされたもので、その
要旨は、Al2O3 9〜20wt％、B2O3 20〜30wt％、SiO2 40
〜60wt％、CaO 3〜15w％、或いはこれらとZrO2 3wt％以
下よりなるガラス被膜を有するガラス被膜窒化アルミニ
ウム焼結体、および窒化アルミニウム焼結体の表面にAl
2O3 9〜20wt％、B2O3 20〜30wt％、SiO2 40〜60wt％、C
aO 3〜15w％、或いはこれらとZrO2 3wt％以下よりなる
ガラス粉末および有機バインダーよって構成されたペー
ストを塗布、加熱してバインダーを除去した後、窒素雰
囲気下、1100〜1500℃の温度で加熱し、次いで冷却して
第１次焼成ガラス層を形成し、さらにその上に上記一次
焼成に使用したガラス粉末および有機バインダーによっ
て構成されたペーストをそれぞれ塗布加熱してバインダ
ーを除去した後、窒素雰囲気下、850〜1100℃に加熱
し、次いで冷却して第２次焼成ガラス層を形成するガラ
ス被覆窒化アルミニウムの製法にある。The present invention has been made to achieve the above object, and its gist is as follows: Al 2 O 3 9 to 20 wt%, B 2 O 3 20 to 30 wt%, SiO 2 40
-60 wt%, CaO 3-15 w%, or a glass-coated aluminum nitride sintered body having a glass coating containing these and ZrO 2 3 wt% or less, and Al on the surface of the aluminum nitride sintered body.
2 O 3 9-20 wt%, B 2 O 3 20-30 wt%, SiO 2 40-60 wt%, C
aO 3-15w%, or a paste composed of glass powder consisting of these and ZrO 2 3wt% or less and an organic binder is applied, heated to remove the binder, and then heated at a temperature of 1100-1500 ° C in a nitrogen atmosphere. Then, it is cooled to form a first-baked glass layer, and the glass powder used for the above-mentioned first-baking and a paste composed of an organic binder are respectively applied and heated thereon to remove the binder, and then a nitrogen atmosphere is applied. Below, it is a method for producing glass-coated aluminum nitride, which is heated at 850-1100 ° C. and then cooled to form a second fired glass layer.

本発明に係るガラス被覆窒化アルミニウム焼結体のガラ
ス組成が上記構成を必須条件とするのは次の理由によ
る。すなわち、Al2O3が9wt％未満では耐湿性が低下し、
20wt％を越えると溶融温度が高くなり、被覆しにくくな
る。B2O3が20wt％未満では溶融温度が高くなりすぎ、30
wt％を越えるとガラスの化学的安定性が低下する。SiO2
が40wt％未満では、ガラスの熱膨張係数と窒化アルミニ
ウム焼結体の熱膨張係数との差が大きく亀裂発生の原因
となり、60wt％を越えると、ガラスの溶融温度が1450℃
以上となり被覆しにくくなる。CaOが、3wt％未満では、
ガラス溶融時の融液の粘性が低くならず均質なガラスが
得られず、15wt％を越えるとガラスの熱膨張係数が窒化
アルミニウム焼結体の熱膨張係数より大きくなり、亀裂
が発生し易くなる。The glass composition of the glass-coated aluminum nitride sintered body according to the present invention has the above-mentioned constitution as an essential condition for the following reason. That is, if Al 2 O 3 is less than 9 wt%, the moisture resistance decreases,
If it exceeds 20 wt%, the melting temperature becomes high and it becomes difficult to coat. If the B 2 O 3 content is less than 20 wt%, the melting temperature will be too high,
If it exceeds wt%, the chemical stability of the glass decreases. SiO 2
If less than 40 wt%, the difference between the coefficient of thermal expansion of the glass and the coefficient of thermal expansion of the aluminum nitride sintered body will be large and cause cracking. If it exceeds 60 wt%, the melting temperature of the glass will be 1450 ℃.
As described above, it becomes difficult to cover. When CaO is less than 3 wt%,
When the glass melts, the viscosity of the melt does not become low and a homogeneous glass cannot be obtained. If it exceeds 15 wt%, the coefficient of thermal expansion of the glass will be larger than that of the aluminum nitride sintered body and cracks will easily occur. .

上記構成のガラスは、室温から380℃の範囲の熱膨張係
数が41〜45×10-7/℃で、窒化アルミニウム焼結体の熱
膨張係数に近似しており、亀裂の発生が防止される。The glass having the above structure has a thermal expansion coefficient in the range of room temperature to 380 ° C. of 41 to 45 × 10 −7 / ° C., which is close to the thermal expansion coefficient of the aluminum nitride sintered body and prevents the occurrence of cracks. .

さらに、ZrO2の添加は、化学的耐久性を向上させる効果
を有するが、3wt％を越えるとガラスが溶融しにくくな
る。Further, addition of ZrO 2 has the effect of improving chemical durability, but if it exceeds 3 wt%, the glass will be difficult to melt.

上記ガラス組成を用いてガラス被覆窒化アルミニウム焼
結体をつくるには、上記割合のAl2O3、B2O3、SiO2、CaO
よりなるガラス粉末、或いはさらにこれにZrO2を添加し
たガラス粉末を有機バインダーと混合し、ガラス粉末が
10〜20wt％含むペーストをつくる。To make a glass-coated aluminum nitride sintered body using the above glass composition, Al 2 O 3 , B 2 O 3 , SiO 2 , and CaO in the above proportions are used.
The glass powder consisting of the above, or the glass powder in which ZrO 2 is further added is mixed with an organic binder, and the glass powder becomes
Make a paste containing 10 to 20 wt%.

これらのペーストのいずれか一方を窒化アルミニウム焼
結体の表面に塗布し、乾燥後、空気中で400℃に加熱し
てバインダーを除去した後、窒素雰囲気下、1100〜1500
℃の温度で加熱し、次いで冷却して均質な第１次焼成ガ
ラス層を形成する。この場合のガラス量は、0.5〜1.0mg
/cm2が適当である。上記加熱温度が1100℃未満では、粘
性が高く、凹部分をうめることが出来ない。1500℃を越
えると、ガラス組成に変化が生じる。Either one of these pastes is applied to the surface of the aluminum nitride sintered body, dried, heated to 400 ° C. in air to remove the binder, and then in a nitrogen atmosphere, 1100 to 1500.
Heat at a temperature of ° C and then cool to form a homogeneous primary fired glass layer. The glass amount in this case is 0.5-1.0 mg
/ cm 2 is suitable. If the heating temperature is less than 1100 ° C, the viscosity is high and the recessed portion cannot be filled. Above 1500 ° C, the glass composition changes.

次に、上記一次焼成ガラス層に用いたものと同じガラス
粉末を、有機バインダーと混合しガラス粉末が50〜60wt
％のペーストをつくる。このペーストを、上記一次焼成
ガラス層が形成された窒化アルミニウム焼結体の表面に
塗布し、乾燥後、空気中で400℃に加熱してバインダー
を除去した後、850〜1100℃の範囲の温度で加熱、冷却
して第２次焼成ガラス層を形成する。上記加熱温度が85
0℃未満ではガラスの溶解が不充分で、1100℃を越える
とガラスの粘性が低下し所定の厚みを得ることができな
い。Next, the same glass powder as that used for the above-mentioned first-baked glass layer was mixed with an organic binder to obtain a glass powder of 50-60 wt.
Make a% paste. This paste is applied to the surface of the aluminum nitride sintered body on which the primary firing glass layer is formed, dried and heated to 400 ° C in air to remove the binder, and then the temperature in the range of 850 to 1100 ° C. And is heated and cooled to form a second fired glass layer. The above heating temperature is 85
If the temperature is lower than 0 ° C, melting of the glass is insufficient, and if the temperature exceeds 1100 ° C, the viscosity of the glass is lowered and a predetermined thickness cannot be obtained.

加熱温度を変えて２層にするのは次の理由による。すな
わち、第１次焼成は窒化アルミニウム焼結体表面にある
凹部分をガラスで被覆するとともに焼結体とガラスとを
反応密着させることを目的とするので、また、第２次焼
成は第１次焼成被膜上に所定の厚みの被膜を形成するた
め、ガラスが流れない温度で焼成する。The reason for changing the heating temperature to two layers is as follows. That is, the primary firing is intended to coat the recessed portion on the surface of the aluminum nitride sintered body with glass and to bring the sintered body and the glass into close contact with each other by reaction. In order to form a coating having a predetermined thickness on the fired coating, firing is performed at a temperature at which glass does not flow.

また、有機バインダーとしては、例えば、エチルセルロ
ーズ、ポリビニルブチラールのような合成樹脂がいずれ
も使用出来るが、一次、二次において使用されるバイン
ダーは必ずしも同じ種類のものでなくてもよい。Further, as the organic binder, for example, synthetic resins such as ethyl cellulose and polyvinyl butyral can be used, but the binders used in the primary and secondary are not necessarily the same kind.

また、塗布方法は、通常行われているスクリーン印刷
法、ドクターブレード法、もしくは刷毛塗り等が採用出
来る。As a coating method, a screen printing method, a doctor blade method, a brush coating method or the like which is commonly used can be adopted.

〔実施例〕〔Example〕

次に、実施例、比較例を示して本発明を説明する。 Next, the present invention will be described with reference to Examples and Comparative Examples.

実施例１、比較例１ 第１表に示すNo.1〜No.7のガラス組成の粉末を粒径10μ
ｍ以下に調整し、有機バインダーと混合してガラス粉末
が58wt％のペーストを作成した。Example 1 and Comparative Example 1 A powder having a glass composition of No. 1 to No. 7 shown in Table 1 had a particle size of 10 μm.
It was adjusted to m or less and mixed with an organic binder to prepare a paste containing 58 wt% of glass powder.

このペーストを窒化アルミニウム焼結体基板の表面に刷
毛で塗布し、乾燥後、空気中で400℃に加熱してバイン
ダーを除去し、次いで、窒素雰囲気下、1200℃または14
00℃の温度でそれぞれ30分間焼成を行なった。得られた
ガラス被覆窒化アルミニウム焼結体のガラス被膜の気
泡、亀裂、乳濁の状態を調べた。その結果を第２表に示
す。 The paste is applied to the surface of the aluminum nitride sintered body substrate with a brush, dried, and heated to 400 ° C in air to remove the binder, and then 1200 ° C or 14 ° C under a nitrogen atmosphere.
Baking was performed for 30 minutes at a temperature of 00 ° C. The glass coating of the obtained glass-coated aluminum nitride sintered body was examined for bubbles, cracks, and emulsions. The results are shown in Table 2.

但し、A:なし、B:微少量、C:少量、D:多量、E:極めて多
量、を示す。（以下同じ）。No.7のガラスは亀裂が多
く、No.1〜No.6は亀裂が生ぜず、また気泡が少ない傾向
にある。 However, A: none, B: very small amount, C: small amount, D: large amount, E: extremely large amount. (same as below). No. 7 glass has many cracks, and No. 1 to No. 6 have no cracks and tend to have few bubbles.

実施例２ 窒化アルミニウム焼結体基板上のガラス被膜の均質性に
ついてNo.2、No.3のガラス組成を用いて粒径10μｍ以下
の粉末を、有機バインダーと混合し、ガラス粉末が10〜
20wt％含有するペーストを調整して、窒化アルミニウム
焼結体基板に塗布量を変えてそれぞれ塗布し、空気中で
400℃に加熱してバインダーを除去した後、窒素雰囲気
下、1400℃で30分加熱し、ガラス被覆窒化アルミニウム
焼結体を作製し、ガラス被膜の不均質性、気泡の状態を
調べた。結果を第３表に示す。Example 2 Regarding homogeneity of glass coating on aluminum nitride sintered body substrate Powders having a particle size of 10 μm or less were mixed with an organic binder by using No. 2 and No. 3 glass compositions, and the glass powder was 10 to 10 μm.
Prepare a paste containing 20 wt% and apply it to the aluminum nitride sintered body substrate at different coating amounts, and in air
After heating to 400 ° C. to remove the binder, heating was performed at 1400 ° C. for 30 minutes in a nitrogen atmosphere to prepare a glass-coated aluminum nitride sintered body, and the inhomogeneity of the glass coating and the state of bubbles were examined. The results are shown in Table 3.

第３表より、不均質性についてはNo.2、No.3共にガラス
の量にかかわらず認められず良好であるが、ガラスの量
が多くなるにつれて気泡発生が増加する。したがって量
は1.0mg/cm2以下が好ましい。 As shown in Table 3, inhomogeneity is good in both No. 2 and No. 3 regardless of the amount of glass, and is good, but as the amount of glass increases, bubble generation increases. Therefore, the amount is preferably 1.0 mg / cm 2 or less.

実施例３ No.2、No.3のガラス組成を用い、２段階焼成法でガラス
被膜の焼成をした。第１次のガラス被膜は基板表面にガ
ラス粉末を10〜20wt％を含むペーストを実施例２と同じ
条件でガラス量を0.5〜1.0mg/cm2となる様に塗布し空気
中で400℃に加熱し、バインダーを除去した後1400℃で3
0分加熱した。第２次焼成は第１次のガラス被膜の表面
に第１次焼成と同じガラス組成でガラス粉末を58wt％を
含むペーストを塗布し、空気中で400℃に加熱してバイ
ンダーを除去した後、1000℃の温度で15分間加熱してガ
ラス被覆を焼成した。この結果均質で亀裂、気泡のない
ガラス被覆を形成することが出来た。Example 3 Using the glass compositions of No. 2 and No. 3, the glass film was fired by the two-step firing method. As the first glass coating, a paste containing 10 to 20 wt% of glass powder was applied to the surface of the substrate under the same conditions as in Example 2 so that the amount of glass was 0.5 to 1.0 mg / cm 2, and the temperature was 400 ° C. in air. After heating and removing the binder, 3 at 1400 ℃
Heated for 0 minutes. In the second firing, a paste containing 58 wt% of glass powder having the same glass composition as that in the first firing is applied to the surface of the first glass coating, heated to 400 ° C. in air to remove the binder, The glass coating was fired by heating at a temperature of 1000 ° C for 15 minutes. As a result, it was possible to form a glass coating that was homogeneous and free of cracks and bubbles.

また、ガラス組成No.1、No.4、No.5、No.6のガラス粉末
についても実施例３と同様に焼成した場合、共に良好な
ガラス被膜を形成することができた。Further, when the glass powders having glass compositions No. 1, No. 4, No. 5, and No. 6 were fired in the same manner as in Example 3, a good glass coating could be formed.

〔効果〕〔effect〕

以上述べたように本発明に係るガラス被覆窒化アルミニ
ウム焼結体は、気泡がなく、均質で膨張係数が窒化アル
ミニウムとほぼ同じで、亀裂の発生のないガラス被膜を
有するので、耐食性の優れた窒化アルミニウム焼結体が
得られる。また、上記ガラス被膜は、第１次および第２
次の焼成ガラス層が順次形成積層されるので、極めて強
固な、ピンホールのないガラス被膜をつくることが出来
る。As described above, the glass-coated aluminum nitride sintered body according to the present invention has no bubbles, is homogeneous and has substantially the same expansion coefficient as aluminum nitride, and since it has a glass coating without cracks, it has excellent corrosion resistance. An aluminum sintered body is obtained. In addition, the above-mentioned glass coating is the first and second
Since the next fired glass layer is sequentially formed and laminated, an extremely strong glass film without pinholes can be formed.

Claims (2)

【特許請求の範囲】[Claims] 【請求項１】Al2O39〜20wt％、B2O320〜30wt％、SiO240
〜60wt％、CaO3〜15wt％、或いはこれらとZrO23wt％以
下よりなるガラス被膜を有することを特徴としたガラス
被覆窒化アルミニウム焼結体。1. Al 2 O 3 9 to 20 wt%, B 2 O 3 20 to 30 wt%, SiO 2 40
~60wt%, CaO3~15wt%, or glass-coated aluminum nitride sintered body characterized by having these glass coatings made of ZrO 2 or less 3 wt%. 【請求項２】窒化アルミニウム焼結体の表面に、Al2O39
〜20wt％、B2O320〜30wt％、SiO240〜60wt％、CaO3〜15
wt％、或いはこれらとZrO23wt％以下よりなるガラス粉
および有機バインダーによって構成されたペーストを塗
布、加熱してバインダーを除去した後、窒素雰囲気下、
1100〜1500℃の温度で加熱し、次いで冷却して第１次焼
成ガラス層を形成し、さらにその上に上記一次焼成に使
用したガラス粉末および有機バインダーによって構成さ
れたペーストをそれぞれ塗布、加熱してバインダーを除
去した後、窒素雰囲気下、850〜1100℃に加熱し、次い
で冷却して第２次焼成ガラス層を形成することを特徴と
したガラス被覆窒化アルミニウムの製法。2. Al 2 O 3 9 is formed on the surface of the aluminum nitride sintered body.
~20wt%, B 2 O 3 20~30wt %, SiO 2 40~60wt%, CaO3~15
wt%, or a paste composed of these and glass powder consisting of ZrO 2 3 wt% or less and an organic binder is applied and heated to remove the binder, and then under a nitrogen atmosphere,
It is heated at a temperature of 1100 to 1500 ° C. and then cooled to form a first-baked glass layer, and the paste composed of the glass powder used for the above-mentioned first-baking and the organic binder is applied and heated thereon. After removing the binder by heating, the mixture is heated to 850 to 1100 ° C. in a nitrogen atmosphere, and then cooled to form a second baked glass layer.
JP62234370A 1987-09-18 1987-09-18 Glass-coated aluminum nitride sintered body and method for producing the same Expired - Lifetime JPH0768065B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62234370A JPH0768065B2 (en) 1987-09-18 1987-09-18 Glass-coated aluminum nitride sintered body and method for producing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62234370A JPH0768065B2 (en) 1987-09-18 1987-09-18 Glass-coated aluminum nitride sintered body and method for producing the same

Publications (2)

Publication Number Publication Date
JPS6479085A JPS6479085A (en) 1989-03-24
JPH0768065B2 true JPH0768065B2 (en) 1995-07-26

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0374636U (en) * 1989-11-16 1991-07-26
JPH0746272B2 (en) * 1989-12-26 1995-05-17 ヤマハ株式会社 Electronic musical instrument
KR20020062308A (en) 1999-12-16 2002-07-25 가부시끼가이샤 도꾸야마 Joint body of glass-ceramic and aluminum nitride sintered compact and method for producing the same
JP2007305508A (en) * 2006-05-15 2007-11-22 Sony Corp Light-emitting device, and light control film
TWI722474B (en) * 2019-07-03 2021-03-21 台灣玻璃工業股份有限公司 Glass materials that increase the weight percentage of boron oxide to reduce the dielectric constant

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JPS6479085A (en) 1989-03-24

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