JPH0117074B2 - - Google Patents
Info
- Publication number
- JPH0117074B2 JPH0117074B2 JP56073721A JP7372181A JPH0117074B2 JP H0117074 B2 JPH0117074 B2 JP H0117074B2 JP 56073721 A JP56073721 A JP 56073721A JP 7372181 A JP7372181 A JP 7372181A JP H0117074 B2 JPH0117074 B2 JP H0117074B2
- Authority
- JP
- Japan
- Prior art keywords
- container
- firing
- silicone resin
- graphite
- thin film
- 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
Links
- 238000010304 firing Methods 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229920002050 silicone resin Polymers 0.000 claims description 12
- 239000010409 thin film Substances 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 description 11
- 239000010408 film Substances 0.000 description 9
- 229910052573 porcelain Inorganic materials 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910004613 CdTe Inorganic materials 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000005376 alkyl siloxane group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- NOKUWSXLHXMAOM-UHFFFAOYSA-N hydroxy(phenyl)silicon Chemical class O[Si]C1=CC=CC=C1 NOKUWSXLHXMAOM-UHFFFAOYSA-N 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Furnace Charging Or Discharging (AREA)
- Light Receiving Elements (AREA)
Description
【発明の詳細な説明】
本発明は基板上に塗布された化合物半導体薄膜
を焼結させる際に用いて最適な焼成用容器に関す
るものであり、特に比較的大面積の基板を熱処理
する場合にその効果を発揮するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sintering container that is most suitable for use in sintering a compound semiconductor thin film coated on a substrate. It is effective.
化合物半導体、たとえばCdSやCdTeなどの焼
結膜は単独で、或は複合層として光導電素子、光
増幅器、光起電力素子などに用いられる。このよ
うな焼結膜は通常CdSなどの高純度微粉末を融剤
としてのCdCl2やその他の微量添加物とともにガ
ラス磁器基板上に塗布、乾燥したのち、N2など
の不活性ガスを主体とした雰囲気中で焼成して作
られる。この場合、融剤としてのCdCl2は高温で
は揮発性があり、雰囲気中のCdCl2濃度が得られ
た焼結膜の性質を左右するので、焼成は通常容器
中で行なわれる。 Sintered films of compound semiconductors, such as CdS and CdTe, are used alone or as composite layers in photoconductive devices, optical amplifiers, photovoltaic devices, and the like. Such sintered films are usually made by coating a high-purity fine powder such as CdS on a glass porcelain substrate together with CdCl 2 as a fluxing agent and other trace additives, drying it, and then applying an inert gas such as N 2 as the main component. It is made by firing in an atmosphere. In this case, the calcination is usually carried out in a container, since CdCl 2 as a flux is volatile at high temperatures and the CdCl 2 concentration in the atmosphere influences the properties of the resulting sintered film.
このような焼成容器としては従来、緻密なアル
ミナ磁器で作られた容器が一般に用いられてい
た。それはアルミナ磁器は焼結膜の特性を損う不
純物が少いこと、腐食性の強いCdCl2蒸気に耐え
ること、空孔率が小さく、汚染されにくいことな
どの理由による。 Conventionally, containers made of dense alumina porcelain have generally been used as such firing containers. This is because alumina porcelain has fewer impurities that impair the properties of the sintered film, can withstand highly corrosive CdCl 2 vapor, has a small porosity, and is less susceptible to contamination.
しかし、基板の寸法が300〜500mm以上の大型基
板を焼成したい場合には、アルミナ磁器製容器に
は次のような大きな問題が発生する。まず、その
ような焼成容器を作ること自体極めて難しく、非
常に高価なものとなる。しかし更に根本的な問題
は、アルミナ磁器が耐熱衝撃性が小さいため、加
熱による破損を避けるためには昇温速度を極端に
遅くせざるを得ず、トンネル炉による焼成の場
合、焼結膜の特性と生産性の両面において相当の
制約を受けるということである。またアルミナ磁
器は熱伝達性が小さいため、容器が大型になると
内部の昇温の遅れが甚しく、焼成すべき基板に精
度の良い熱処理を加えることが難しいばかりでな
く、基板の中央部と周辺部とで甚だしい焼成むら
が起り、特性の不均一となつてあらわれることも
大きな問題である。そのほか容器の寸法精度をあ
げにくいとか、重量が大となり、取扱いにくいと
いうような問題も発生する。 However, when it is desired to fire a large substrate with dimensions of 300 to 500 mm or more, the following major problems occur with the alumina porcelain container. First, making such a firing container itself is extremely difficult and extremely expensive. However, a more fundamental problem is that alumina porcelain has low thermal shock resistance, so the temperature increase rate must be extremely slow to avoid damage due to heating, and when firing in a tunnel furnace, the characteristics of the sintered film This means that there are considerable constraints in terms of both productivity and productivity. In addition, alumina porcelain has low heat conductivity, so when the container becomes large, there is a significant delay in temperature rise inside the container, which not only makes it difficult to apply accurate heat treatment to the substrate to be fired, but also makes it difficult to heat the substrate in the center and surrounding areas. Another major problem is that severe unevenness in firing occurs between parts, resulting in non-uniform properties. Other problems arise, such as difficulty in improving the dimensional accuracy of the container, and the increased weight of the container, making it difficult to handle.
本発明はこのような点に鑑みて成されたもので
あり、上記した問題点を除去した焼成用容器を提
供するものである。本発明の焼成用容器は黒鉛を
用いて作られており、さらにその表面の必要部分
にはケイ素樹脂の炭化物の薄膜が設けられている
ことを特徴とするものである。この薄膜が目的と
するところは、黒鉛微粉の脱落による半導体焼結
膜の汚染の防止と焼成用容器の耐久性の向上にあ
る。本発明の焼成用容器の形状は図面にその断面
を示すように、浅い箱形の容器１と、それにゆる
く嵌合する蓋２より成る。蓋２には必要により１
個またはそれ以上の細孔３を設ける。また４はケ
イ素樹脂炭化物薄膜であつて、容器の内部底面を
除く全表面を被覆した例を示す。５は焼成用基板
である。この場合、容器１の内部底面は焼成用基
板５でそのほとんどが覆われてしまうので、ケイ
素樹脂炭化物薄膜４で内部底面が被覆されていな
くても、焼成用基板５の上面に形成されている化
合物半導体薄膜などが汚染されるようなことはな
い。黒鉛は熱伝導性、耐熱衝撃性ともアルミナ磁
器にくらべ桁ちがいに大きく、また硬度が高くな
いため機械加工は容易で寸法精度も出しやすく、
更にCdCl2などに対する耐蝕性も大きいというす
ぐれた特長をもつている。また耐酸化性について
もCdSの焼成が行なわれる600℃程度までは十分
あるが、通常CdS焼成はN2を主体とするガス中
で行なわれるため全く問題は起らない。しかし、
黒鉛の容器は取扱いの際に微粉が付着したり加
熱・冷却の過程で微粉が脱落したりする危険を伴
うので、本発明のケイ素樹脂炭化物の被覆がこの
ような問題発生防止に極めて有効である。 The present invention has been made in view of these points, and it is an object of the present invention to provide a baking container that eliminates the above-mentioned problems. The firing container of the present invention is made of graphite, and is further characterized in that a thin film of carbide of silicone resin is provided on necessary portions of its surface. The purpose of this thin film is to prevent contamination of the semiconductor sintered film due to shedding of fine graphite powder and to improve the durability of the firing container. The shape of the baking container of the present invention, as shown in its cross section in the drawing, consists of a shallow box-shaped container 1 and a lid 2 that fits loosely therein. 1 for lid 2 as necessary
or more pores 3 are provided. Reference numeral 4 shows an example in which a silicone resin carbide thin film covers the entire surface of the container except for the inner bottom surface. 5 is a substrate for firing. In this case, most of the internal bottom surface of the container 1 is covered with the baking substrate 5, so even if the internal bottom surface is not covered with the silicone resin carbide thin film 4, it is formed on the top surface of the baking substrate 5. There is no possibility of contamination of compound semiconductor thin films. Graphite has much higher thermal conductivity and thermal shock resistance than alumina porcelain, and because it is not hard, it is easy to machine and achieve dimensional accuracy.
Furthermore, it has the excellent feature of high corrosion resistance against substances such as CdCl 2 . In addition, the oxidation resistance is sufficient up to about 600°C, which is the temperature at which CdS is fired, but normally CdS is fired in a gas mainly composed of N2 , so no problems occur. but,
Graphite containers carry the risk of fine powder adhering to them when handled or falling off during heating and cooling processes, so the silicone resin carbide coating of the present invention is extremely effective in preventing such problems from occurring. .
本発明の焼成用容器は黒鉛ブロツクからの機械
的加工によるほか、コークス微粒子とピツチとの
〓合物を加圧成型したのち、焼成、ピツチ含浸、
焼成、黒鉛化したのち、表面被覆する方法によつ
ても製造することが出来る。 The baking container of the present invention is produced not only by mechanical processing from a graphite block, but also by pressure-molding a mixture of fine coke particles and pitch, followed by baking, pitch impregnation, and so on.
It can also be produced by a method in which the surface is coated after firing and graphitizing.
ケイ素樹脂炭化物による被覆する方法として
は、アルキルシロキサン系やフエニルシロキサン
系のケイ素樹脂の有機溶剤による希薄溶液を塗布
するが、溶液中に黒鉛製容器を浸漬したのち乾燥
し、硬化に必要な温度に加熱し、次に窒素などの
不活性雰囲気中で、800℃ないし1200℃程度の高
温で熱処理することが推奨される。このような処
理により、黒鉛表面に炭素、ケイ素および酸素を
主成分とするシリコカーボンと呼ばれるケイ素樹
脂の炭化物の薄膜が形成されると、容器に接触し
た時、黒鉛微粉末が付着したり、また、加熱・冷
却の過程で黒鉛微粉末が脱落したりすることは全
くなくなる。なお、ケイ素樹脂炭化物薄膜は膜厚
が極めて小さくても十分その効果を発揮する。ま
たこのような処理により、黒鉛の表面層の気孔が
ケイ素樹脂炭化物で充填されるため、焼成中に発
生するCdCl2蒸気が空孔中に拡散し、蓄積するの
を軽減することが出来る。 The method of coating with silicone resin carbide is to apply a dilute solution of alkylsiloxane-based or phenylsiloxane-based silicone resin in an organic solvent, but after immersing a graphite container in the solution, it is dried and then heated to the temperature required for curing. It is recommended to heat the material to 800°C to 1200°C in an inert atmosphere such as nitrogen. Through such treatment, a thin film of carbide of silicon resin called silicocarbon, whose main components are carbon, silicon, and oxygen, is formed on the graphite surface, and when it comes into contact with the container, fine graphite powder may adhere or This eliminates the possibility of fine graphite powder falling off during the heating and cooling process. Note that even if the silicone resin carbide thin film has an extremely small thickness, it can sufficiently exhibit its effects. Furthermore, by such treatment, the pores in the surface layer of graphite are filled with silicone resin carbide, so that it is possible to reduce the diffusion and accumulation of CdCl 2 vapor generated during firing into the pores.
次に、本発明の一実施例について述べる。 Next, an embodiment of the present invention will be described.
空孔率15％、灰分含有率1200ppmの黒鉛ブロツ
クを機械加工して外形寸法が360×360×45mmで、
図面に示すような形状とした。次にケイ素樹脂ワ
ニス（トーレ・シリコーン(株)製、SH805）をキシ
レンで希釈し、樹脂分が５％としたものを上記の
容器の表面に薄く塗布し、120℃で１時間乾燥し
たのち、温度を250℃に上げさらに２時間加熱し
た。次にこれを窒素ガス中で徐々に昇温し、1100
℃で２時間保つたのち冷却し、図面と同一の構造
の焼成用容器を作製した。 Machined from a graphite block with a porosity of 15% and an ash content of 1200ppm, the external dimensions are 360 x 360 x 45 mm.
The shape was as shown in the drawing. Next, silicone resin varnish (manufactured by Toray Silicone Co., Ltd., SH805) was diluted with xylene, and a resin content of 5% was applied thinly to the surface of the container, and after drying at 120°C for 1 hour, The temperature was raised to 250°C and heated for an additional 2 hours. Next, gradually raise the temperature in nitrogen gas to 1100
After being kept at ℃ for 2 hours, it was cooled to produce a firing container having the same structure as the drawing.
次に、99.99％の純度のCdS微粉末100ｇ、
CdCl210ｇ、プロピレングリコール30ｇよりなる
ペーストをスクリーン印刷法により300×300×３
mmのホウケイ酸ガラス基板上に塗布し、120℃で
３時間乾燥した。この基板を上記の焼成用容器に
入れ、全長４ｍのトンネル炉を通過させた。最高
温度は650℃、雰囲気はN299％、O21％であつた。
この焼成条件により得られたCdS焼結膜は黄色半
透明であり、導電性が大きくCdS−Cu2S系およ
びCdS−CdTe系太陽電池用として適することが
わかつた。 Next, 100g of CdS fine powder with 99.99% purity,
A paste consisting of 10 g of CdCl 2 and 30 g of propylene glycol was printed 300 x 300 x 3 using the screen printing method.
It was coated on a borosilicate glass substrate (mm) and dried at 120°C for 3 hours. This substrate was placed in the above-mentioned firing container and passed through a tunnel furnace having a total length of 4 m. The maximum temperature was 650°C, and the atmosphere was 99% N 2 and 1% O 2 .
It was found that the CdS sintered film obtained under these firing conditions was yellow and semitransparent, had high conductivity, and was suitable for use in CdS-Cu 2 S-based and CdS-CdTe-based solar cells.
比較のため上記実施例において、ケイ素樹脂炭
化物被覆を行なわず他は実施例と同一条件とした
場合には、容器の取扱いの際に手が黒く汚れ、ま
た得られたCdS焼結膜の面にはところどころに褐
色や黒色の斑点があらわれ、その部分は光透過率
や導電性が不十分で上記の太陽電池用として適当
でないことがわかつた。 For comparison, in the above example, when the silicone resin carbide coating was not performed and the other conditions were the same as in the example, hands were stained black when handling the container, and the surface of the obtained CdS sintered film was Brown or black spots appeared here and there, and it was found that these areas had insufficient light transmittance and conductivity, and were therefore unsuitable for the above-mentioned solar cell.
以上の説明から明らかなように本発明による焼
成用容器を用いることにより、大面積ですぐれた
特性の化合物半導体薄膜が得られる。なお、上記
実施例においてはCdS膜の焼成について記したが
本発明の焼成用容器はCdSe、CdTe、ZnS、
ZnSeあるいはそれらの固溶体についても同様に
適用することができる。 As is clear from the above description, by using the firing container according to the present invention, a compound semiconductor thin film with a large area and excellent properties can be obtained. In addition, although the above embodiment describes the firing of CdS film, the firing container of the present invention can be used for CdSe, CdTe, ZnS,
The same can be applied to ZnSe or solid solutions thereof.
図面は本発明の焼成用容器の一実施例を示す断
面図である。
１……容器本体、２……蓋、３……小孔、４…
…ケイ素樹脂の炭化物の薄膜、５……焼成すべき
基板。
The drawing is a sectional view showing one embodiment of the baking container of the present invention. 1... Container body, 2... Lid, 3... Small hole, 4...
... Thin film of carbide of silicone resin, 5 ... Substrate to be fired.
Claims (1)
ゆるく嵌合する同材質の蓋とからなり、前記容器
の内部底面を除く内壁面および外壁面と、前記蓋
の内側表面および外側表面とが、ケイ素樹脂の炭
化物の薄膜で被膜されていることを特徴とする焼
成用容器。1 Consisting of a shallow box-shaped container made of graphite and a lid made of the same material that fits loosely into the container, the inner and outer wall surfaces of the container, excluding the inner bottom surface, and the inner and outer surfaces of the lid are , a firing container characterized by being coated with a thin film of silicone resin carbide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56073721A JPS57188822A (en) | 1981-05-15 | 1981-05-15 | Vessel for baking |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56073721A JPS57188822A (en) | 1981-05-15 | 1981-05-15 | Vessel for baking |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57188822A JPS57188822A (en) | 1982-11-19 |
| JPH0117074B2 true JPH0117074B2 (en) | 1989-03-28 |
Family
ID=13526365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56073721A Granted JPS57188822A (en) | 1981-05-15 | 1981-05-15 | Vessel for baking |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57188822A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0228395Y2 (en) * | 1981-06-15 | 1990-07-30 | ||
| JPH07116715B2 (en) * | 1992-01-10 | 1995-12-13 | 建設省北陸地方建設局長 | Retaining wall construction method |
-
1981
- 1981-05-15 JP JP56073721A patent/JPS57188822A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57188822A (en) | 1982-11-19 |
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