JPH0818917B2 - Method for producing CdTe single crystal - Google Patents
Method for producing CdTe single crystalInfo
- Publication number
- JPH0818917B2 JPH0818917B2 JP2210277A JP21027790A JPH0818917B2 JP H0818917 B2 JPH0818917 B2 JP H0818917B2 JP 2210277 A JP2210277 A JP 2210277A JP 21027790 A JP21027790 A JP 21027790A JP H0818917 B2 JPH0818917 B2 JP H0818917B2
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- heat treatment
- single crystal
- temperature
- resistivity
- 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 - Fee Related
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- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
- Light Receiving Elements (AREA)
- Measurement Of Radiation (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 発明の技術分野 本発明は、放射線検出素子用等として有用な高抵抗Cd
Te単結晶の製造方法に関する。Description: TECHNICAL FIELD OF THE INVENTION The present invention relates to a high resistance Cd useful as a radiation detection element and the like.
The present invention relates to a method for manufacturing a Te single crystal.
従来技術 CdTe単結晶は放射線検出素子等に有用であり、その特
性向上、特に高エネルギー分解能化をめざして従来から
CdTe単結晶の製造方法が検討されている。Conventional technology CdTe single crystal is useful for radiation detectors, etc.
A method for producing a CdTe single crystal has been studied.
高エネルギー分解能を達成するための結晶特性として
は、主に次の２点が重要である。The following two points are important as crystal characteristics for achieving high energy resolution.
第１点は、抵抗率が高いことである。抵抗率が低いと
放射線検出器の信号ノイズが増大し好ましくなく、１×
108Ωcm以上の値が必要である。第２点はキャリアライ
フタイムが大きいことである。キャリアライフタイムが
小さいと、キャリア収集効率が低下し、エネルギー分解
能が低下する。The first point is that the resistivity is high. If the resistivity is low, the signal noise of the radiation detector increases, which is not preferable, and 1 ×
A value of 10 8 Ωcm or more is required. The second point is that the carrier lifetime is long. When the carrier lifetime is short, the carrier collection efficiency is lowered and the energy resolution is lowered.
以上のことから、放射線検出素子用の結晶の製造条件
の検討は、高抵抗率化、キャリアライフタイムの増大の
２点に注目して行なわれてきた。From the above, the examination of the manufacturing conditions of the crystal for the radiation detection element has been conducted by paying attention to two points, that is, high resistivity and increase of carrier lifetime.
第１点目の高抵抗率化に対しては、結晶成長時にClを
ドープして抵抗率を向上する事が報告されている。Regarding the first point, that of increasing the resistivity, it has been reported that Cl is doped during the crystal growth to improve the resistivity.
第２点目のキャリアライフタイムの増大に関しては、
結晶の純度の向上によって達成される事が報告されてい
る。Regarding the second point, the increase in career lifetime,
It has been reported to be achieved by improving the purity of crystals.
本発明が解決する問題点 従来から、高抵抗率の結晶を得るためには、結晶中に
添加する塩素濃度を高めることにより効果があることが
知られている。しかし、塩素濃度が高くなるほどキャリ
アライフタイムは低下する傾向があるため、放射線検出
素子に適した充分抵抗率が高く、しかもキャリアライフ
タイムも大きい結晶を得ることが出来ないという問題点
があった。すなわち、放射線検出素子として使用可能な
抵抗率を得るためには、塩素の添加量をある程度大きな
量にせざるを得ない。そのため、キャリアライフタイム
が小さくなり、結果的に、この結晶を使用して作製した
放射線検出素子のエネルギー分解能は満足できる値を得
ることができないという問題があった。Problems to be Solved by the Invention It has been conventionally known that increasing the concentration of chlorine added to the crystal is effective for obtaining a crystal having a high resistivity. However, since the carrier lifetime tends to decrease as the chlorine concentration increases, there is a problem in that it is not possible to obtain a crystal having a sufficiently high resistivity suitable for a radiation detection element and a long carrier lifetime. That is, in order to obtain a resistivity that can be used as a radiation detection element, the amount of chlorine added must be increased to some extent. Therefore, the carrier lifetime becomes small, and as a result, there is a problem that a satisfactory value cannot be obtained for the energy resolution of the radiation detection element manufactured using this crystal.
発明の構成 本発明は、上記の問題点を解決したものであって、放
射線検出素子用のCdTe単結晶の製造方法において、得ら
れる単結晶中の塩素濃度が0.8重量ppm以上５重量ppm以
下となるように塩素源を添加し、単結晶の成長後、350
℃以上450℃以下の温度で15時間以上の熱処理をした
後、段階的に温度を下げながら熱処理を行なうことを特
徴とするCdTe単結晶の製造方法に関するものである。The present invention is to solve the above-mentioned problems, and in the method for producing a CdTe single crystal for a radiation detecting element, the chlorine concentration in the obtained single crystal is 0.8 wtppm or more and 5 wtppm or less. Add a chlorine source so that after growing a single crystal, 350
The present invention relates to a method for producing a CdTe single crystal, which comprises performing heat treatment for 15 hours or more at a temperature of ℃ or more and 450 ℃ or less, and then performing heat treatment while gradually lowering the temperature.
問題点を解決する手段および作用 上記の問題点を解決するためには、低塩素濃度でも抵
抗率の高い結晶を得る方法が必要であり、本発明者等
は、結晶を成長した後の冷却過程において、350℃以上4
50℃以下の温度で15時間以上の熱処理をした後、段階的
に温度を下げながら熱処理することで抵抗率が増加する
ことを新たに見い出し、本発明に至ったものである。Means and Actions for Solving Problems In order to solve the above problems, a method for obtaining a crystal having a high resistivity even at a low chlorine concentration is necessary, and the present inventors have proposed a cooling process after growing the crystal. At 350 ℃ or above 4
The present invention has been newly found that the resistivity is increased by performing heat treatment at a temperature of 50 ° C. or lower for 15 hours or more and then performing heat treatment while gradually lowering the temperature.
本発明におけCdTeの結晶成長方法とは、トラベリング
ヒーター法、ブリッジマン法、グラジエントフリージン
グ法等の方法であって、塩素源を添加して行う結晶成長
法の殆ど全てを含む。The CdTe crystal growth method in the present invention is a method such as a traveling heater method, a Bridgman method, a gradient freezing method or the like, and includes almost all the crystal growth methods performed by adding a chlorine source.
本発明における、塩素源としては、CdCl2,TeCl4,TeCl
2,Cl2等である。これは、CdTeの抵抗率を高めるために
添加される。添加量は、結晶成長方法及びその条件によ
って異なるが、CdTe結晶中の塩素濃度が0.8重量ppm以
上、５重量ppm以下となるように添加する。0.8重量ppm
未満では、本発明の結晶成長後に引き続き行われる熱処
理を行っても、第１図に示すごとく、放射線検出素子に
使用可能な１×108Ωcm以上の抵抗率にならないため好
ましくない。また、５重量ppmを超える場合は、第２図
に示すごとく、キャリアライフタイムが低下するため
に、エネルギー分解能が低下し好ましくない。In the present invention, as the chlorine source, CdCl 2 , TeCl 4 , TeCl
2 , Cl 2, etc. It is added to increase the resistivity of CdTe. The addition amount varies depending on the crystal growth method and the conditions thereof, but it is added so that the chlorine concentration in the CdTe crystal is 0.8 weight ppm or more and 5 weight ppm or less. 0.8 weight ppm
If it is less than the above value, the heat treatment subsequently performed after the crystal growth of the present invention does not result in a resistivity of 1 × 10 8 Ωcm or more which can be used for the radiation detecting element, as shown in FIG. 1, which is not preferable. On the other hand, if it exceeds 5 ppm by weight, as shown in FIG. 2, the carrier lifetime is reduced and the energy resolution is reduced, which is not preferable.
本発明の熱処理は、結晶成長終了後の室温まで冷却す
る過程で行う。したがって、これは、結晶成長を行った
アンプル等の容器の中に入ったまま行われる。このた
め、結晶の取扱いによる汚染を極めて少なくすることが
できる。特にウェハーにした後に熱処理を行なう方法に
比べて汚染が少ない。The heat treatment of the present invention is performed in the process of cooling to room temperature after completion of crystal growth. Thus, this is done while still in a container such as an ampoule where the crystal has grown. Therefore, the contamination caused by handling the crystal can be extremely reduced. In particular, the contamination is less than that of the method in which a heat treatment is performed after forming the wafer.
また、この時の熱処理は450℃以下の温度域に対して
行われる。450℃を越える温度域で熱処理しても、抵抗
率の向上にはなんら寄与しない。また、この時の450℃
とは結晶の温度であって、炉の温度ではない。したがっ
て、結晶が勾配のある温度分布の中にあるときは、炉の
温度が450℃を越える温度であっても、結晶の１部が450
℃以下になったときに本発明の熱処理が始まる。The heat treatment at this time is performed in a temperature range of 450 ° C. or lower. Heat treatment in the temperature range over 450 ° C does not contribute to the improvement of resistivity. Also, at this time 450 ℃
Is the temperature of the crystal, not the temperature of the furnace. Therefore, when the crystal is in a gradient temperature distribution, even if the temperature of the furnace exceeds 450 ° C, a part of the crystal is 450
The heat treatment of the present invention starts when the temperature falls below the temperature of ° C.
第３図に示すごとく、冷却速度が50℃/hrを越えると
と抵抗率が放射線検出素子に使用可能な１×108Ωcmよ
り小さくなるため、好ましくない。特に結晶中の塩素濃
度が１〜2ppm前後と小さい場合は、更に冷却速度を小さ
くする必要がある。好ましくは20℃/hr以下の冷却速度
とする。As shown in FIG. 3, if the cooling rate exceeds 50 ° C./hr, the resistivity becomes smaller than 1 × 10 8 Ωcm usable for the radiation detecting element, which is not preferable. Especially when the chlorine concentration in the crystal is as low as 1 to 2 ppm, it is necessary to further reduce the cooling rate. The cooling rate is preferably 20 ° C./hr or less.
本発明の熱処理の方法は、第４図に示すごとく、350
℃以上450℃以下の温度で15時間以上の熱処理をした
後、段階的に温度を下げながら熱処理を行なうことであ
る。350℃以上450℃以下の温度で15時間以上の熱処理を
行なうことにより、結晶中の抵抗率のばらつきが小さく
なるとともに、その平均値も向上する。350℃以上450℃
以下の温度で熱処理をしたあと、できるだけ低温まで熱
処理を行うことが、より高い抵抗率が得られるため好ま
しい。例えば、380℃、300℃、200℃、100℃と段階的に
熱処理を変えていくことが好ましい。As shown in FIG. 4, the heat treatment method of the present invention is performed at 350
This is to perform heat treatment for 15 hours or more at a temperature of ℃ or more and 450 ℃ or less, and then perform heat treatment while gradually lowering the temperature. By performing the heat treatment at a temperature of 350 ° C. or higher and 450 ° C. or lower for 15 hours or longer, the variation in resistivity in the crystal is reduced and the average value thereof is also improved. 350 ° C or more 450 ° C
It is preferable to perform heat treatment at the following temperature and then heat treatment to a temperature as low as possible because a higher resistivity can be obtained. For example, it is preferable to gradually change the heat treatment at 380 ° C, 300 ° C, 200 ° C, and 100 ° C.
［参考例］ Teを溶媒とし、結晶中の塩素濃度が２重量ppmになる
ようにCdCl2を塩素源として添加し、トラベリングヒー
ター法で、CdTe単結晶を製造後、10℃/hrの冷却速度で
降温した後、この結晶を用いて放射線検出素子を作製し
た。[Reference example] Te was used as a solvent, and CdCl 2 was added as a chlorine source so that the chlorine concentration in the crystal was 2 ppm by weight, and a CdTe single crystal was produced by the traveling heater method, and then the cooling rate was 10 ° C / hr. After the temperature was lowered at, a radiation detecting element was produced using this crystal.
この結晶の抵抗率は、３×108Ωcm、キャリアライフ
タイムは電子が0.65μs,ホールが0.35μｓと高抵抗、高
キャリアライフタイムを同時に満足するものであった。The resistivity of this crystal was 3 × 10 8 Ωcm, the carrier lifetime was 0.65 μs for electrons and 0.35 μs for holes, and both high resistance and high carrier lifetime were satisfied at the same time.
放射線検出素子としての特性は、241Amの放射線（59.
5keVのエネルギーをもっている）を測定したときのピー
ク強度半値幅が、印加電圧15Vにおいて6keVの良好な分
解能が得られた。The characteristics as a radiation detection element are the radiation of 241 Am (59.
When the applied voltage was 15V, the resolution was 6keV.
［実施例］ 第５図に示すごとく、Teを溶媒とし、結晶中の塩素濃
度が２重量ppmになるようにCdCl2を塩素源として添加
し、図中結晶成長炉１で、トラベリングヒーター法で、
CdTe単結晶を成長した後、引き続き、図中熱処理炉２に
アンプル３を移動し、第４図に示すように温度を段階的
に下げながら、熱処理を行った。この結晶を用いて放射
線検出素子を作製した。[Example] As shown in FIG. 5, Te was used as a solvent, and CdCl 2 was added as a chlorine source so that the chlorine concentration in the crystal would be 2 ppm by weight. ,
After growing the CdTe single crystal, the ampoule 3 was subsequently moved to the heat treatment furnace 2 in the figure, and heat treatment was performed while gradually lowering the temperature as shown in FIG. A radiation detection element was produced using this crystal.
この結晶の抵抗率は、４×108Ωcm、キャリアライフ
タイムは電子が0.65μs,ホールが0.35μｓと高抵抗、高
キャリアライフタイムを同時に満足するものであった。The resistivity of this crystal was 4 × 10 8 Ωcm, and the carrier lifetime was 0.65 μs for electrons and 0.35 μs for holes, and both high resistance and high carrier lifetime were satisfied at the same time.
放射線検出素子としての特性は、241Amの放射線（59.
5keVのエネルギーをもっている）を測定したときのピー
ク強度半値幅が、印加電圧15Vにおいて5keVの良好な分
解能が得られた。The characteristics as a radiation detection element are the radiation of 241 Am (59.
When the applied voltage was 15V, the resolution of the peak intensity half width was 5keV.
［比較例］ Teを溶媒とし、結晶中の塩素濃度が２重量ppmになる
ようにCdCl2を塩素源として添加し、トラベリングヒー
ター法で、CdTe単結晶を成長後、150℃/hrの冷却速度で
降温したあと、この結晶を用いて放射線検出素子を作製
した。[Comparative Example] Te was used as a solvent, CdCl 2 was added as a chlorine source so that the chlorine concentration in the crystal was 2 ppm by weight, and a CdTe single crystal was grown by the traveling heater method, and then the cooling rate was 150 ° C / hr. After the temperature was lowered at, a radiation detecting element was produced using this crystal.
この結晶の抵抗率は、５×105Ωcmであり、キャリア
ライフタイムは抵抗値が低すぎたため、測定できなかっ
た。The resistivity of this crystal was 5 × 10 5 Ωcm, and the carrier lifetime could not be measured because the resistance value was too low.
放射線検出素子としての特性は、抵抗率が低すぎたた
めに、リーク電流が大きく、241Amの放射線を測定した
ところ、なんらスペクトルが得られなかった。Regarding the characteristics of the radiation detection element, the resistivity was too low, so the leak current was large, and when a radiation of 241 Am was measured, no spectrum was obtained.
発明の効果 本発明により、結晶中塩素濃度が0.8重量ppm以上５重
量ppm以下という低塩素濃度でも、放射線検出素子を作
製するのに充分な抵抗率の高い結晶を得ることが出来
る。このため、この結晶を用いて、従来よりもエネルギ
ー分解能の良好な放射線検出素子を作製することができ
る。EFFECTS OF THE INVENTION According to the present invention, it is possible to obtain a crystal having a sufficiently high resistivity for producing a radiation detecting element even when the chlorine concentration in the crystal is as low as 0.8 weight ppm or more and 5 weight ppm or less. Therefore, by using this crystal, it is possible to manufacture a radiation detection element having a better energy resolution than ever before.
第１図は結晶中の塩素濃度と本発明の熱処理によって得
られた抵抗率の関係を示したものである。 第２図は結晶中の塩素濃度とキャリアライフタイムの関
係を示したものである。 第３図は冷却速度と抵抗率の関係を示したものである。 第４図は段階的に熱処理温度を下げる場合の一例を示し
たものであって、実施例における熱処理条件である 第５図は実施例における、結晶成長装置を示したもので
ある。 １……結晶成長炉 ２……熱処理炉 ３……アンプル ４……CdTe単結晶 ５……Te溶媒 ６……原料CdTe多結晶FIG. 1 shows the relationship between the chlorine concentration in the crystal and the resistivity obtained by the heat treatment of the present invention. FIG. 2 shows the relationship between the chlorine concentration in the crystal and the carrier lifetime. FIG. 3 shows the relationship between the cooling rate and the resistivity. FIG. 4 shows an example of the case where the heat treatment temperature is lowered stepwise, and shows the heat treatment conditions in the embodiment. FIG. 5 shows the crystal growth apparatus in the embodiment. 1 ... Crystal growth furnace 2 ... Heat treatment furnace 3 ... Ampule 4 ... CdTe single crystal 5 ... Te solvent 6 ... Raw material CdTe polycrystal
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｌ 31/0248 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Internal reference number FI technical display location H01L 31/0248
Claims (1)
において、得られる単結晶中の塩素濃度が0.8重量ppm以
上５重量ppm以下となるように塩素源を添加し、単結晶
の成長後、350℃以上450℃以下の温度で15時間以上の熱
処理をした後、段階的に温度を下げながら熱処理を行な
うことを特徴とするCdTe単結晶の製造方法。1. A method for producing a CdTe single crystal for a radiation detecting element, wherein a chlorine source is added so that the chlorine concentration in the obtained single crystal is 0.8 weight ppm or more and 5 weight ppm or less, and after the growth of the single crystal. A method for producing a CdTe single crystal, which comprises performing heat treatment at a temperature of 350 ° C. or higher and 450 ° C. or lower for 15 hours or more, and then performing the heat treatment while gradually lowering the temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2210277A JPH0818917B2 (en) | 1990-08-10 | 1990-08-10 | Method for producing CdTe single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2210277A JPH0818917B2 (en) | 1990-08-10 | 1990-08-10 | Method for producing CdTe single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0497991A JPH0497991A (en) | 1992-03-30 |
| JPH0818917B2 true JPH0818917B2 (en) | 1996-02-28 |
Family
ID=16586730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2210277A Expired - Fee Related JPH0818917B2 (en) | 1990-08-10 | 1990-08-10 | Method for producing CdTe single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0818917B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06345598A (en) * | 1993-06-04 | 1994-12-20 | Japan Energy Corp | CdTe crystal for radiation detection element and manufacturing method thereof |
| JP3448688B2 (en) | 1998-05-11 | 2003-09-22 | 株式会社ジャパンエナジー | CdTe crystal or CdZnTe crystal and method for producing the same |
| JP6018532B2 (en) * | 2013-03-29 | 2016-11-02 | Ｊｘ金属株式会社 | Semiconductor wafer, radiation detection element, radiation detector, and method for producing compound semiconductor single crystal |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5338596A (en) * | 1976-09-20 | 1978-04-08 | Riken Vitamin Oil Co Ltd | Process for formula feed for larvae and juveniles of fish and shellfishes |
-
1990
- 1990-08-10 JP JP2210277A patent/JPH0818917B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0497991A (en) | 1992-03-30 |
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