JP6332573B1 - 電界効果型トランジスタ、その製造方法、それを用いた無線通信装置および商品タグ - Google Patents
電界効果型トランジスタ、その製造方法、それを用いた無線通信装置および商品タグ Download PDFInfo
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- JP6332573B1 JP6332573B1 JP2017560829A JP2017560829A JP6332573B1 JP 6332573 B1 JP6332573 B1 JP 6332573B1 JP 2017560829 A JP2017560829 A JP 2017560829A JP 2017560829 A JP2017560829 A JP 2017560829A JP 6332573 B1 JP6332573 B1 JP 6332573B1
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Abstract
Description
(ポリシロキサン)
本発明におけるゲート絶縁層は、ポリシロキサンを含有し、少なくとも、一般式(1)で表される構造単位を有する。
一般式(1)において、R1は、水素原子、アルキル基、シクロアルキル基、複素環基、アリール基、ヘテロアリール基又はアルケニル基を表す。R2は、水素原子、アルキル基、シクロアルキル基又はシリル基を表す。mは0又は1を表す。A1は、カルボキシル基、スルホ基、チオール基、フェノール性水酸基又はそれらの誘導体を少なくとも二つ含む有機基を表す。ただし、前記誘導体が、前記カルボキシル基、スルホ基、チオール基およびフェノール性水酸基のうちの二つによる環状縮合構造である場合は、A1は当該環状縮合構造を少なくとも一つ有する有機基を表す。
ヒステリシスとは、電圧履歴に対する電流値の変動幅を表しており、FETの安定駆動のためには、ヒステリシスの値を小さくする必要がある。ヒステリシスは、20V以下が好ましく、10V以下がより好ましく、5V以下がさらに好ましい。
本発明に用いられる一般式(1)で表される構造単位を有するポリシロキサンは、例えば次の方法で得ることができる。溶媒中に全シラン化合物を溶解し、ここに酸触媒および水を1〜180分かけて添加した後、15〜80℃で1〜180分加水分解反応させる。加水分解反応時の温度は、15〜55℃がより好ましい。この反応液を、50℃以上、溶媒の沸点以下で1〜100時間加熱し、縮合反応を行うことにより、一般式(1)で表される構造単位を有するポリシロキサンを得ることができる。
本発明におけるゲート絶縁層は、FETのしきい値電圧とヒステリシス低減の観点から、金属原子と酸素原子の結合を含む金属化合物を含むことが好ましい。金属化合物は、金属原子と酸素原子の結合を含むものであれば特に制限はなく、例えば金属酸化物、金属水酸化物等が例示される。金属化合物に含まれる金属原子は、金属キレートを形成するものであれば特に限定されないが、マグネシウム、アルミニウム、チタン、クロム、マンガン、コバルト、ニッケル、銅、亜鉛、ガリウム、ジルコニウム、ルテニウム、パラジウム、インジウム、ハフニウム、白金などが挙げられる。中でも、入手容易性、コスト、金属キレートの安定性の点からアルミニウムが好ましい。
なお、ゲート絶縁層における原子(炭素原子、ケイ素原子、金属原子)の含有比率の関係は大まかな傾向であり、例えば金属原子の種類等によっては必ず上述の関係が満たされるわけではない。
ベンゾフェノン系光重合開始剤としては、例えば、ベンゾフェノン、4,4’−ビス(ジメチルアミノ)ベンゾフェノン、4,4’−ビス(ジエチルアミノ)ベンゾフェノン、4−フェニルベンゾフェノン、4,4−ジクロロベンゾフェノン、4−ヒドロキシベンゾフェノン、アルキル化ベンゾフェノン、3,3’,4,4’−テトラキス(t−ブチルパーオキシカルボニル)ベンゾフェノン、4−メチルベンゾフェノン、ジベンジルケトン又はフルオレノンが挙げられる。
芳香族ケトエステル系光重合開始剤としては、例えば、2−フェニル−2−オキシ酢酸メチルが挙げられる。
連鎖移動剤を含むことで、UV光の照射時の感度を向上させることができる。これは、UV光の照射によって発生したラジカルが、連鎖移動剤によって他のポリマー鎖へラジカル移動することで、膜の深部にまでラジカル架橋をするためであると推測される。
重合禁止剤を適量含有させることで、UV光照射時に発生する過剰量のラジカルを抑制し、ラジカル重合を制御することができる。
本発明の実施の形態に係るFETは、後述の半導体層に対してゲート絶縁層と反対側に第2絶縁層を有してもよい。ここで、半導体層に対してゲート絶縁層と反対側とは、例えば、半導体層の上側にゲート絶縁層を有する場合は半導体層の下側を指す。これにより、しきい値電圧やヒステリシスを低減することができ、高性能なFETが得られる。第2絶縁層に用いられる材料としては特に限定されないが、具体的には酸化シリコン、アルミナ等の無機材料、ポリイミドやその誘導体、ポリビニルアルコール、ポリビニルクロライド、ポリエチレンテレフタレート、ポリフッ化ビニリデン、ポリシロキサンやその誘導体、ポリビニルフェノールやその誘導体等などのポリマー材料、あるいは無機材料粉末とポリマー材料の混合物や有機低分子材料とポリマー材料の混合物を挙げることができる。ポリシロキサンを含む絶縁層としては、本発明におけるゲート絶縁層も含まれる。これらの中でも、インクジェット等の塗布法で作製できるポリマー材料を用いることが好ましい。特に、ポリフルオロエチレン、ポリノルボルネン、ポリシロキサン、ポリイミド、ポリスチレン、ポリカーボネート又はこれらの誘導体、ポリアクリル酸誘導体、ポリメタクリル酸誘導体、又はこれらを含む共重合体を用いると、しきい値電圧及びヒステリシス低減効果がより大きくなるため好ましく、ポリアクリル酸誘導体、ポリメタクリル酸誘導体、又はこれらを含む共重合体が特に好ましい。
半導体層に用いられる材料は、有機半導体及び/又はカーボン材料である。これらは、キャリア移動度の高い材料が好ましく用いられ、また、低コストで簡便な塗布プロセスが適用できる点で好ましい。
半導体層は単層でも複数層でもよく、膜厚は1nm以上200nm以下が好ましく、100nm以下がさらに好ましい。この範囲の膜厚にすることにより、均一な薄膜形成が容易になり、さらにゲート電圧によって制御できないソース・ドレイン間電流を抑制し、FETのオンオフ比をより高くすることができる。膜厚は、原子間力顕微鏡やエリプソメトリ法などにより測定できる。
基板に用いる材料としては、少なくとも電極系が配置される面が絶縁性であればいかなる材質のものでもよい。例えば、シリコンウェハー、ガラス、サファイア、アルミナ焼結体等の無機材料、ポリイミド、ポリビニルアルコール、ポリビニルクロライド、ポリエチレンテレフタレート、ポリフッ化ビニリデン、ポリシロキサン、ポリビニルフェノール(PVP)、ポリエステル、ポリカーボネート、ポリスルホン、ポリエーテルスルホン、ポリエチレン、ポリフェニレンスルフィド、ポリパラキシレン等の有機材料などが好適に用いられる。
また、例えばシリコンウェハー上にPVP膜を形成したものや、ポリエチレンテレフタレート上にポリシロキサン膜を形成したものなど、複数の材料が積層されたものであってもよい。
ゲート電極、ソース電極及びドレイン電極に用いる材料としては、例えば、酸化錫、酸化インジウム、酸化錫インジウム(ITO)などの導電性金属酸化物;白金、金、銀、銅、鉄、錫、亜鉛、アルミニウム、インジウム、クロム、リチウム、ナトリウム、カリウム、セシウム、カルシウム、マグネシウム、パラジウム、モリブデン、アモルファスシリコンやポリシリコンなどの金属やこれらの合金;ヨウ化銅、硫化銅などの無機導電性物質;ポリチオフェン、ポリピロール、ポリアニリン;ポリエチレンジオキシチオフェンとポリスチレンスルホン酸の錯体;ヨウ素などのドーピングなどで導電率を向上させた導電性ポリマーなど;炭素材料などの導電体などが挙げられる。これらの材料は、単独で用いてもよいが、複数の材料を積層又は混合して用いてもよい。
中でも、銀、銅、金、白金、鉛、錫、ニッケル、アルミニウム、タングステン、モリブデン、酸化ルテニウム、クロム、チタン、カーボン若しくはインジウムの少なくとも1種を含む導電性粉末の焼結体が好ましく、これらの導電性粉末は単独、合金、あるいは混合粉末として用いることができる。
体積平均粒子径が0.1μm以上であると導電性粉末同士の接触確率が向上し、作製される導電パターンの比抵抗値、及び断線確率を低くすることができる。さらに、露光時の活性光線が膜中をスムーズに透過することができるため、微細なパターニングが容易となる。
なお、体積平均粒子径は、電極断面の3D−走査型電子顕微鏡(SEM)や3D−透過型電子顕微鏡(TEM)像から算出することができる。
有機バインダーを有することで、電極上における半導体溶液の塗布性が向上し、有機半導体及びカーボン材料が平滑に塗布された均一な半導体層を形成することが可能になる。また、有機バインダーが感光性有機成分を含むことで、レジストを用いずフォトリソグラフィーによる電極のパターン加工ができ、より生産性を向上させることが可能になる。
分子内に重合性不飽和基を有するモノマーとしては、活性な炭素−炭素不飽和二重結合を有する化合物を用いることができる。官能基として、ビニル基、アリル基、アクリレート基、メタクリレート基、アクリルアミド基を有する単官能及び多官能化合物が応用できる。
このような側鎖をオリゴマーもしくはポリマーに付加させる方法は、オリゴマーもしくはポリマー中のメルカプト基、アミノ基、水酸基やカルボキシル基に対して、グリシジル基やイソシアネート基を有するエチレン性不飽和化合物やアクリル酸クロライド、メタクリル酸クロライド又はアリルクロライドを付加反応させて作る方法がある。また、グリシジル基やイソシアネート基を有するエチレン性不飽和化合物やアクリル酸クロライド、メタクリル酸クロライド又はアリルクロライドは、オリゴマーもしくはポリマー中のメルカプト基、アミノ基、水酸基やカルボキシル基に対して0.05モル等量〜1モル等量付加させることが好ましい。
光重合開始剤と共に増感剤を使用することで感度を向上させ、反応に有効な波長範囲を拡大することができる。
図1及び図2は、本発明の実施の形態に係るFETの例を示す模式断面図である。図1では、ゲート絶縁層3で覆われたゲート電極2を有する基板1上に、ソース電極5及びドレイン電極6が形成された後、さらにその上に半導体層4が形成されている。図2では、ゲート絶縁層3で覆われたゲート電極2を有する基板1上に半導体層4が形成された後、さらにその上にソース電極5及びドレイン電極6が形成されている。
μ=(δId/δVg)L・D/(W・εr・ε・Vsd) (a)
ただしId(A)はソース電極5とドレイン電極6との間の電流、Vsd(V)はソース電極5とドレイン電極6との間の電圧、Vg(V)はゲート電圧(ゲート電極2の電圧)、D(m)はゲート絶縁層3の厚み、L(m)はチャネル長(ソース電極5とドレイン電極6との距離)、W(m)はチャネル幅(ソース電極5、ドレイン電極6の幅)、εrはゲート絶縁層3の比誘電率、εは真空の誘電率(8.85×10−12F/m)である。
ヒステリシスは、Vgを正から負へと印加した際のId=10−8Aにおけるゲート電圧Vg1と、Vgを負から正へと印加した際のId=10−8Aにおけるゲート電圧Vg2との差の絶対値|Vg1−Vg2|から求めることができる。
しきい値電圧は、Id−Vgグラフにおける線形部分の延長線とVg軸との交点から求めることができる。また、Vg=−20Vにおけるゲート電流値をリーク電流とした。
本発明の実施の形態に係るFETの製造方法は、
(I)基板上に導電性パターンを形成する工程、
(II)少なくとも、一般式(1)で表される構造単位を有するポリシロキサンを含む溶液を、上記導電性パターンが形成された基板上に塗布及び乾燥する工程、
(III)有機半導体及び/又はカーボン材料を含む溶液を、導電性パターンに接するように塗布及び乾燥する工程、
を含む。
(I)基板上に導電性パターンを形成する工程、
(II−A)少なくとも、一般式(1)で表される構造単位を有するポリシロキサン、および感光性有機成分を含む溶液を、前記導電性パターンが形成された基板上に塗布及び乾燥し得られた膜に、フォトマスクを介して活性化学線を照射した後、アルカリ溶液を用いて、前記導電性パターン上に開口部となるパターンを形成する工程、
(II−B)前記パターンを加熱して、硬化パターンを形成する工程、
(III)有機半導体及び/又はカーボン材料を含む溶液を、導電性パターンに接するように塗布及び乾燥する工程、
を含むことが好ましい。
本発明の実施の形態に係るFETを含有する無線通信装置について説明する。この無線通信装置は、例えば、非接触型タグであるRFID(Radio Frequency IDentification)のような、リーダ/ライタに搭載されたアンテナから送信される搬送波を受信することで電気通信を行う装置である。具体的な動作は、例えばリーダ/ライタに搭載されたアンテナから送信された無線信号を、RFIDタグのアンテナが受信し、整流回路により直流電流に変換されRFIDタグが起電する。次に、起電されたRFIDタグは、無線信号からコマンドを受信し、コマンドに応じた動作を行う。その後、コマンドに応じた結果の回答をRFIDタグのアンテナからリーダ/ライタのアンテナへ無線信号を送信する。なお、コマンドに応じた動作は少なくとも公知の復調回路、動作制御ロジック回路、変調回路で行われる。
本発明の実施の形態に係る無線通信装置を含有する商品タグについて説明する。この商品タグは、例えば基体と、この基体によって被覆された上記無線通信装置を有している。
基体は、例えば、平板状に形成された紙などの非金属材料によって形成されている。例えば、基体は2枚の平板状の紙を貼り合わせた構造をしており、この2枚の紙の間に上記無線通信装置が配置されている。上記無線記憶装置の記憶回路に、例えば商品を個体識別する個体識別情報が予め格納されている。
6インチシリコンウェハー及び6インチガラス基板上に、ゲート絶縁層材料をスピンコーターを用いて、乾燥後の膜厚が0.5μmとなるように塗布し、ついでホットプレ−ト(大日本スクリーン製造(株)製SCW−636)を用いて、120℃で3分乾燥し、コーティング膜を得た。
感光性を有する材料を含まないゲート絶縁層材料について、以下の方法でゲート絶縁層を作製した。上記(1)で作製した6インチシリコンウェハー及び6インチガラス基板上のコーティング膜を、所定の温度、時間で加熱処理することにより、ゲート絶縁層を得た。
感光性を有する材料を含むゲート絶縁層材料の内、光ラジカル発生剤とラジカル重合性化合物を含有する材料について、以下の方法でゲート絶縁層を作製した。上記(1)記載の方法で作製した6インチシリコンウェハー及び6インチガラス基板上に形成されたコーティング膜を、i線ステッパー(GCA製DSW−8000)にセットし、100〜800mJ/cm2の露光量にてコーティング膜の上方から所望のパターンを有するネガ型マスクを通して露光した。露光後、90℃のホットプレートで1分間PEBを行い、2.38質量%の水酸化テトラメチルアンモニウム(TMAH)水溶液(三菱ガス化学(株)製、ELM−D)で60秒現像し、ついで純水でリンスした。この膜を、所定の温度、時間で加熱処理することにより、ゲート絶縁層を得た。
感光性を有する材料を含むゲート絶縁層材料の内、光酸発生剤としてジアゾケトン化合物を含有する材料について、以下の方法でゲート絶縁層を作製した。上記(1)記載の方法で作製した6インチシリコンウェハー及び6インチガラス基板上に形成されたコーティング膜を、i線ステッパーにセットし、100〜800mJ/cm2の露光量にてコーティング膜の上方から所望のパターンを有するポジ型マスクを通して露光した。露光後、2.38質量%のTMAH水溶液で60秒現像し、ついで純水でリンスした。この膜を、所定の温度、時間で加熱処理することにより、ゲート絶縁層を得た。
光干渉式膜厚測定装置であるラムダエースSTM−602(大日本スクリーン製造(株)製)を使用し、屈折率1.55で基板上の面内10点を測定し、その算術平均をゲート絶縁層の厚さとして求めた。
測定したい膜に超高真空中において軟X線を照射し、表面から放出される光電子を検出するX線光電子分光(PHI社製 Quantera SXM)により膜中の元素情報、元素量を分析した。
接触角計(協和界面科学(株)製、CA−D型)を使用し、室温下で直径1.5mmの、半導体溶液の液滴を針先に作り、これを、上記(2)−1、(2)−2、(2)−3に記載の方法で作製した6インチシリコンウェハー上のゲート絶縁層に触れさせて、液滴を作った。この時に生ずる液滴と面との角度を測定し、接触角とした。これを下記のように判定し、A、B及びCを半導体溶液の塗布性良好につき合格とした。
A:接触角が6°以上10°未満
B:接触角が5°以上6°未満又は10°以上12°未満
C:接触角が4°以上5°未満又は12°以上15°未満
D:接触角が3°以上4°未満又は15°以上20°未満
E:接触角が3°未満又は20°以上。
後述する膜厚50nmで線幅20μmのゲート電極パターン上に塗布形成した上で、窒素気流下200℃で30分間加熱処理を施し得られたゲート絶縁層を光学顕微鏡で観察し、電極近傍から生じるクラックの発生率を素子ごとの観察結果の総計から算出し、「100−(クラック発生率%)」を耐クラック性の指標とした。これを下記のように判定し、A、B及びCをゲート絶縁層の耐クラック性良好につき合格とした。
A:耐クラック性が100%
B:耐クラック性が98%以上100%未満
C:耐クラック性が94%以上98%未満
D:耐クラック性が91%以上95%未満
E:耐クラック性が91%未満。
FETを得た後に、ゲート電圧(Vg)を変えたときのソース・ドレイン間電流(Id)−ソース・ドレイン間電圧(Vsd)特性を測定した。測定には半導体特性評価システム4200−SCS型(ケースレーインスツルメンツ(株)製)を用い、大気中(気温20℃、湿度35%)で測定した。Vgを正から負へと印加した際のId=10−8Aにおけるゲート電圧Vg1と、Vgを負から正へと印加した際のId=10−8Aにおけるゲート電圧Vg2との差の絶対値|Vg1−Vg2|から、ヒステリシスを求めた。これを下記のように判定し、A、B及びCを低ヒステリシスにつき合格とした。
A:ヒステリシスが5V以下
B:ヒステリシスが5Vより大きく、10V以下
C:ヒステリシスが10Vより大きく、20V以下
D:ヒステリシスが20Vより大きく、30V以下
E:ヒステリシスが30Vより大きい。
また、Vg=−20Vにおけるゲート電流値からリーク電流を求めた。これを下記のように判定し、A、B及びCを低リーク電流につき合格とした。
A :リーク電流が10pA以下
B+:リーク電流が10pAより大きく、15pA以下
B :リーク電流が15pAより大きく、20pA以下
C+:リーク電流が20pAより大きく、25pA以下
C :リーク電流が25pAより大きく、30pA以下
D :リーク電流が30pAより大きく、50pA以下
E :リーク電流が50pAより大きい。
上記(2)−2、(2)−3記載の方法により作製した6インチシリコンウェハー上のコーティング膜について、光学顕微鏡のラムダエースSTM−602を用いて、感度及び解像度を評価した。なお、100μmのラインアンドスペースパターンを1対1の幅に形成する露光量(以下、最適露光量という)を感度とし、最適露光量における現像後に得られた最小パターン寸法を解像度とした。これを下記のように判定し、A、B及びCをパターン解像性良好につき合格とした。
A:解像度が5μm以下
B:解像度が5μmより大きく、15μm以下
C:解像度が15μmより大きく、30μm以下
D:解像度が30μmより大きく、45μm以下
E:解像度が45μmより大きい。
(1)半導体溶液Aの作製
ポリ−3−ヘキシルチオフェン(アルドリッチ社製、レジオレギュラー、数平均分子量(Mn):13000、以下P3HTという)0.10gをクロロホルム5mlの入ったフラスコの中に加え、超音波洗浄機(井内盛栄堂(株)製US−2、出力120W)中で超音波撹拌することによりP3HTのクロロホルム溶液を得た。次いでこの溶液をスポイトにとり、メタノール20mlと0.1規定塩酸10mlの混合溶液の中に0.5mlずつ滴下して、再沈殿を行った。固体になったP3HTを0.1μm孔径のメンブレンフィルター(PTFE社製:4フッ化エチレン)によって濾別捕集し、メタノールでよくすすいだ後、真空乾燥により溶媒を除去した。さらにもう一度溶解と再沈殿を行い、90mgの再沈殿P3HTを得た。
3−トリメトキシシリルプロピルコハク酸無水物(SucSi)13.12g(0.05モル)、3−アクリロキシプロピルトリメトキシシラン(AcrSi)93.73g(0.40モル)およびフェニルトリメトキシシラン(PheSi)109.06g(0.55モル)をプロピレングリコールモノメチルエーテルアセテート(PGMEA、沸点146℃)215.91gに溶解し、これに、水54.90g、リン酸0.864gを撹拌しながら加えた。得られた溶液をバス温105℃で2時間加熱し、内温を90℃まで上げて、主として副生するメタノールからなる成分を留出せしめた。次いでバス温130℃で2時間加熱し、内温を118℃まで上げて、主として水とメタノールからなる成分を留出せしめた後、室温まで冷却し、固形分濃度26.0質量%のポリシロキサン溶液Aを得た。得られたポリシロキサン溶液Aを10gはかり取り、PGMEA0.83gを混合して、室温にて2時間撹拌し、絶縁層材料溶液A(固形分濃度24質量%)を得た。
図1に示すFETを作製した。ガラス製の基板1(膜厚0.7mm)上に、抵抗加熱法により、マスクを通して金を50nm真空蒸着し、ゲート電極2を形成した。次に作製した絶縁層材料溶液Aをゲート電極2が形成された基板1上にスピンコート塗布(800rpm×20秒)し、120℃で3分間熱処理後、窒素気流下200℃で30分間熱処理することによって、膜厚400nmのゲート絶縁層3を形成した。次に、抵抗加熱法により、金を膜厚50nmになるように真空蒸着し、その上にフォトレジスト(商品名「LC100−10cP」、ローム・アンド・ハース(株)製)をスピンコート塗布(1000rpm×20秒)し、100℃で10分加熱乾燥した。作製したフォトレジスト膜をパラレルライトマスクアライナー(キヤノン(株)製PLA−501F)を用いて、マスクを介してパターン露光した後、自動現像装置(滝沢産業(株)製AD−2000)を用いて2.38質量%水酸化テトラメチルアンモニウム水溶液であるELM−D(商品名、三菱ガス化学(株)製)で70秒間シャワー現像し、次いで水で30秒間洗浄した。その後、AURUM−302(商品名、関東化学(株)製)で5分間エッチング処理した後、水で30秒間洗浄した。AZリムーバ100(商品名、メルクパフォーマンスマテリアルズ(株)製)に5分間浸漬してレジストを剥離し、水で30秒間洗浄後、120℃で20分間加熱乾燥することでソース電極5およびドレイン電極6を形成した。
実施例1で作成したポリシロキサン溶液Aを10gはかり取り、DPHA(商品名「KAYARAD」、日本化薬(株)製;ジペンタエリスリトールヘキサアクリレート)を1.04g、OXE−01(商品名「イルガキュア」、BASFジャパン(株)製)を0.15gとPGMEA4.60gを混合して、室温にて2時間撹拌し、絶縁層材料溶液B(固形分濃度24質量%)を得た。絶縁層材料溶液B中のDPHAの含有量は、ポリシロキサン60質量部に対して40質量部であった。また、絶縁層材料溶液B中のOXE−01の含有量は、ポリシロキサン60質量部に対して3.5質量部であった。感光性有機成分を含む絶縁層材料溶液Bを用い、前記「(2)−2 ゲート絶縁層の作製(b)」に従い、それ以外は実施例1と同様にゲート絶縁層3およびFETを作製し、評価した。
表1に示す絶縁層材料溶液C〜O、半導体溶液A及び電極材料(Au)を用い、実施例2と同様にしてFETを作製し、評価した。
SucSiに代わり、3−トリメトキシシリルプロピルグルタル酸無水物(GltSi)を用いた絶縁層材料溶液Pを使用する以外は、実施例10と同様にしてFETを作製し、評価した。
GltSiに代わり、3−(3−トリメトキシシリルプロピロキシ)プロパン−1,2−ジチオール(DMrcSi)を用いた絶縁層材料溶液Qを使用する以外は、実施例16と同様にしてFETを作製し、評価した。
DPHAとOXE−01を添加せずに、固形分濃度24質量%の絶縁層材料溶液Rを使用した点以外は、実施例17と同様にしてFETを作製し、評価した。
ポリシロキサン溶液Aを用い、これを10gはかり取り、DPHAを1.04g、OXE−01を0.15g、アルミニウムトリス(2,4−ペンタンジオナート)(商品名「アルミキレートA(W)」、川研ファインケミカル(株)製、以下、AlA(W)という)を1.35gとPGMEA7.53gを混合して、室温にて2時間撹拌し、絶縁層材料溶液S(固形分濃度24質量%)を得た。絶縁層材料溶液S中の上記AlA(W)の含有量は、ポリシロキサン及びDPHAの合計100質量部に対して28質量部であった。絶縁層材料溶液Sを用い、実施例2と同様にゲート絶縁層3およびFETを作製し、評価した。
半導体溶液の調製時、P3HTを用いずにCNTのみの溶液を用意し、これを半導体溶液Bとして半導体層4の形成に用いる以外は、実施例19と同様にゲート絶縁層3およびFETを作製し、評価した。
半導体溶液の調製時、CNTを用いずにP3HTのみの溶液を用意し、これを半導体溶液Cとして半導体層4の形成に用いる以外は、実施例19と同様にゲート絶縁層3およびFETを作製し、評価した。
電極の作製を、感光性有機成分を含む導電性ペーストにて、以下のように行った。
100mlクリーンボトルにアクリルポリマーSPCR−69X(商品名、昭和電工(株)製、重量平均分子量15000)を20g、光重合開始剤OXE−01(BASFジャパン(株)製)4g、酸発生剤SI−110(三新化学工業(株)製)を0.6g、γ−ブチロラクトン(三菱ガス化学(株)製)を10g入れ、自転−公転真空ミキサー“あわとり練太郎”(登録商標)(ARE−310;(株)シンキー製)で混合し、感光性樹脂溶液46.6g(固形分78.5質量%)を得た。得られた感光性樹脂溶液8.0gと平均粒子径2μmのAg粒子を42.0g混ぜ合わせ、3本ローラー“EXAKT M−50”(商品名、EXAKT社製)を用いて混練し、50gの感光性Agペーストを得た。
感光性Agペーストをスクリーン印刷でガラス製の基板1上に塗布し、乾燥オーブンで100℃、10分でプリベークを行った。その後、露光装置“PEM−8M”(商品名、ユニオン光学(株)製)を用いて、電極に対応するマスクパターンを有するフォトマスクを介して露光量70mJ/cm2(波長365nm換算)で全線露光を行い、0.5%Na2CO3溶液で30秒間浸漬現像を行い、超純水でリンス後、乾燥オーブンで140℃、30分間キュアを行い、ゲート電極2を作製した。同様の手順にて、ソース電極5及びドレイン電極6も作製した。これら以外は実施例19と同様にゲート絶縁層3およびFETを作製し、評価した。
始めに光酸発生剤の合成を、以下のように行った。
乾燥窒素気流下、Ph−cc−AP−MF(商品名、本州化学工業(株)製)15.32g(0.05mol)と5−ナフトキノンジアジドスルホニル酸クロリド37.62g(0.14mol)を1,4−ジオキサン450gに溶解させ、室温にした。ここに、1,4−ジオキサン50gと混合させたトリエチルアミン15.58g(0.154mol)を系内が35℃以上にならないように滴下した。滴下後30℃で2時間撹拌した。トリエチルアミン塩を濾過し、濾液を水に投入した。その後、析出した沈殿を濾過で集めた。この沈殿を真空乾燥機で乾燥させ、ジアゾナフトキノン化合物(QD−01、4−[1−(4−ヒドロキシフェニル)−1−フェニルエチル]−1,2−ベンゼンジオールと6−ジアゾ−5,6−ジヒドロ−5−オキソ−ナフタレン−1−スルホン酸との(モノ〜トリ)エステル)を得た。
次にポリシロキサン溶液Aを用い、これを10gはかり取り、QD−01を1.19g、AlA(W)を1.38gとPGMEA7.53gを混合して、室温にて2時間撹拌し、絶縁層材料溶液Z(固形分濃度24質量%)を得た。絶縁層材料溶液Z中の上記AlA(W)の含有量は、ポリシロキサン及びQD−01の合計100質量部に対して28質量部であった。絶縁層材料溶液Zを用い、前記「(2)−3 ゲート絶縁層の作製(c)」に従いゲート絶縁層3を作製した後、実施例22と同様にFETを作製し、評価した。
SucSi及びAcrSiに代わり、3−トリメトキシシリルプロピルチオール(MrcSi)0.45モルを用いた絶縁層材料溶液Tを使用する以外は、実施例1と同様にしてFETを作製し、評価した。
SucSi及びAcrSiに代わり、MrcSiを0.45モル用いた絶縁層材料溶液Uを使用する以外は、実施例2と同様にしてFETを作製し、評価した。
2 ゲート電極
3 ゲート絶縁層
4 半導体層
5 ソース電極
6 ドレイン電極
10 アンテナ
Claims (16)
- 少なくとも、基板と、ソース電極、ドレイン電極及びゲート電極と、前記ソース電極及びドレイン電極に接する半導体層と、前記半導体層を前記ゲート電極と絶縁するゲート絶縁層と、を備えた電界効果型トランジスタであって、
前記半導体層が、有機半導体及び/又はカーボン材料を含有し、
前記ゲート絶縁層が、少なくとも、下記一般式(1)で表される構造単位を有するポリシロキサンを含有することを特徴とする、電界効果型トランジスタ。
- 前記一般式(1)におけるA1が、カルボキシル基又はその誘導体を少なくとも二つ、若しくは環状の酸無水物基を少なくとも一つ有する有機基である、請求項1に記載の電界効果型トランジスタ。
- 前記ポリシロキサンは、全シラン構造単位に対して前記一般式(1)で表される構造単位を0.5mol%以上20mol%以下の割合で含有する、請求項1〜3のいずれかに記載の電界効果型トランジスタ。
- 前記ポリシロキサンは、全シラン構造単位に対して前記一般式(4)で表される構造単位を5mol%以上50mol%以下の割合で含有する、請求項5に記載の電界効果型トランジスタ。
- 前記半導体層が、カーボンナノチューブを含む、請求項1〜6のいずれかに記載の電界効果型トランジスタ。
- 前記カーボンナノチューブが、カーボンナノチューブ表面の少なくとも一部に共役系重合体が付着したカーボンナノチューブ複合体を含む、請求項7に記載の電界効果型トランジスタ。
- 前記ソース電極、ドレイン電極及び/又はゲート電極が、有機バインダー及び導電体を含む、請求項1〜8のいずれかに記載の電界効果型トランジスタ。
- 前記ゲート絶縁層が、金属原子と酸素原子の結合を含む金属化合物を含有する、請求項1〜9のいずれかに記載の電界効果型トランジスタ。
- 請求項1〜10のいずれかに記載の電界効果型トランジスタの製造方法であって、
(I)基板上に導電性パターンを形成する工程、
(II)少なくとも、一般式(1)で表される構造単位を有するポリシロキサンを含む溶液を、前記導電性パターンが形成された基板上に塗布及び乾燥する工程、
(III)有機半導体及び/又はカーボン材料を含む溶液を、導電性パターンに接するように塗布及び乾燥する工程、
を含む、電界効果型トランジスタの製造方法。 - (I)基板上に導電性パターンを形成する工程、
(II−A)少なくとも、一般式(1)で表される構造単位を有するポリシロキサン、および感光性有機成分を含む溶液を、前記導電性パターンが形成された基板上に塗布及び乾燥し得られた膜に、フォトマスクを介して活性化学線を照射した後、アルカリ溶液を用いて、前記導電性パターン上に開口部となるパターンを形成する工程、
(II−B)前記パターンを加熱して、硬化パターンを形成する工程、
(III)有機半導体及び/又はカーボン材料を含む溶液を、導電性パターンに接するように塗布及び乾燥する工程、
を含む、請求項11に記載の電界効果型トランジスタの製造方法。 - 前記感光性有機成分が、光によりラジカルを発生する化合物及びラジカル重合性化合物を含む、請求項12に記載の電界効果型トランジスタの製造方法。
- 前記感光性有機成分が、光により酸を発生する化合物を含む、請求項12に記載の電界効果型トランジスタの製造方法。
- 請求項1〜10のいずれかに記載の電界効果型トランジスタを有する無線通信装置。
- 請求項15に記載の無線通信装置を用いた商品タグ。
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