JPH03150357A - Target and production thereof - Google Patents
Target and production thereofInfo
- Publication number
- JPH03150357A JPH03150357A JP1288524A JP28852489A JPH03150357A JP H03150357 A JPH03150357 A JP H03150357A JP 1288524 A JP1288524 A JP 1288524A JP 28852489 A JP28852489 A JP 28852489A JP H03150357 A JPH03150357 A JP H03150357A
- Authority
- JP
- Japan
- Prior art keywords
- target
- powder
- density
- wox
- mold
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000007731 hot pressing Methods 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 3
- 150000004767 nitrides Chemical class 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 3
- 150000001247 metal acetylides Chemical class 0.000 claims 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims 1
- 238000004544 sputter deposition Methods 0.000 abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011163 secondary particle Substances 0.000 abstract description 3
- 239000010409 thin film Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000012856 packing Methods 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 2
- 229910052581 Si3N4 Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 239000011224 oxide ceramic Substances 0.000 abstract 1
- 229910052574 oxide ceramic Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 6
- 238000001272 pressureless sintering Methods 0.000 description 5
- 238000005566 electron beam evaporation Methods 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 208000003464 asthenopia Diseases 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、例えばエレクトロクロミック現象を利用した
表示素子を得るためのスパッタリング又は電子ビーム蒸
着用成膜原料となるターゲットとその製造方法に関する
。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a target that is a film forming material for sputtering or electron beam evaporation to obtain a display element that utilizes an electrochromic phenomenon, for example, and a method for manufacturing the same.
表示素子等の中、エレクトロクロミック表示素子は、液
晶に比べてはるかに鮮明で、長時間使用しても目の疲れ
が少なく、また少し斜めから見ると表示が見えにくくな
るという液晶特有の視覚依存性もないことから、大型デ
ィスプレイ、ディジタル時計、電卓等に、液晶に代わる
次世代の表示素子として開発が進められ、−ａＩＳＳ品
化されている。Among display elements, electrochromic display elements are much clearer than liquid crystals, cause less eye fatigue even when used for long periods of time, and have visual dependence unique to liquid crystals, which makes the display difficult to see when viewed from a slight angle. Because of its lack of flexibility, it is being developed as a next-generation display element to replace liquid crystals in large displays, digital watches, calculators, etc., and is being turned into an -aISS product.
現在開発が進められているエレクトロクロミック表示素
子の多くはＷＯヨ（Ｘ≦３．０）薄膜を用いたものであ
り、この薄膜はＷＯ，の常圧焼結により製造された成形
体を成膜原料（ターゲット）として用い、スパッタリン
グ又は電子ビーム蒸着により得られる。Many of the electrochromic display elements currently under development use WO (X≦3.0) thin films, and these thin films are formed by forming compacts manufactured by pressureless sintering of WO. It is used as a raw material (target) and obtained by sputtering or electron beam evaporation.
しかし、このエレクトロクロミック表示素子が液晶等の
従来の表示素子に取って代わるためには、表示素子とし
ての諸特性とともに製造コストの低減も大きな解決課題
となる。However, in order for this electrochromic display element to replace conventional display elements such as liquid crystals, reduction of manufacturing costs as well as various characteristics as a display element are major issues to be solved.
この製品原価のコストにおいては、ＷＯ，の原料費が大
きな部分を占めてふり、エレクトロクロミック表示素子
の低価格化並びに成膜性能の観点から、前述ターゲット
の消耗率の低減とターゲット表面が均一に消耗すること
が強く望まれている。In the cost of this product, the raw material cost of WO accounts for a large part, and from the viewpoint of lowering the price of electrochromic display elements and film forming performance, it is possible to reduce the consumption rate of the target mentioned above and to make the target surface uniform. It is strongly desired to be consumed.
ところが、従来のＷＯ，ターゲットは常圧焼結により製
造されており、ターゲットの消耗量が多く、また、消耗
が均一に進まないため短時間で使用できなくなり、また
、５０ｍｍ径を越える比較的大型の成形体は焼結中に割
れを生じ易く、内部構造が緻密で均一な成形体を安定し
て製造するのは困難であった。However, conventional WO targets are manufactured by pressureless sintering, which causes a large amount of target wear, and the wear does not progress uniformly, making the target unusable in a short period of time. The molded bodies were prone to cracking during sintering, and it was difficult to stably produce molded bodies with a dense and uniform internal structure.
この高密度を達成する方法の一つとして、ホットプレス
の適用が考えられるが、通常のホットプレスではカーボ
ンモールドが使用され、また保温材としてカーボン粉末
又はカーボン繊維が使用される等、還元雰囲気が強いた
め、高温で還元されやすいＷＯｓ の成形体を通常のホ
ットプレスで得ることは困難である。One way to achieve this high density is to apply hot pressing, but in normal hot pressing, a carbon mold is used, and carbon powder or carbon fiber is used as a heat insulator, etc. in a reducing atmosphere. Because of its strength, it is difficult to obtain molded bodies of WOs, which are easily reduced at high temperatures, by ordinary hot pressing.
本発明（Ｄターｒ ｙ ） Ｉｔ、ＷＯ，ｌ（Ｘ＝２．
０〜３．０）の均一な組成を有し、ターゲットの表面の
均一な消耗を達成し、且つ消耗量を減少させるために高
密度としたものである。The present invention (Dterry) It, WO, l (X=2.
It has a uniform composition of 0 to 3.0) and has a high density to achieve uniform abrasion of the target surface and reduce the amount of abrasion.
これまでの常圧焼結で製造されたターゲットは、これを
構成する結晶粒の集合体、いわゆる２次粒子の間に多く
の空隙を有しており、このため、ターゲット表面の均一
な消耗が達成されなかった。Targets manufactured by conventional pressureless sintering have many voids between the aggregates of crystal grains that make up the target, so-called secondary particles, and this prevents uniform wear of the target surface. Not achieved.
本発明のターゲットは、ホットプレスを採用することに
より、これら２次粒子間の空隙を極めて少なくし、均一
な消耗を可能にした。By employing hot pressing, the target of the present invention minimizes the voids between these secondary particles and enables uniform consumption.
表１にターゲットの密度及び焼成方法と、電子ビーム蒸
着におけるターゲットの消耗の均一性の関係を示す。こ
れより、密度が６゜Ｏｇ ／ ｃｄ以上で均一な消耗が
可能であることが判る。Table 1 shows the relationship between target density, firing method, and uniformity of target consumption during electron beam evaporation. From this, it can be seen that uniform consumption is possible when the density is 6° Og/cd or more.
表１：ターゲットの密度と消耗の均一性ｉ密度ｇ／ｃｄ
ｌ焼成方法Ｉ消耗の均一性ｌｌｌｉｔｏ 常圧焼
結 ｘ １６１５．２ １ ＃ ｌ
Δ １１８１５．７ １ ホット
プレス １ Δ １１９＋５．
８ 常圧焼結１ Δ Ｉ１１０１ ６．
０ １ 本フＦプＪ ｌ
ｏ Ｈ１１１１６，２１〃ｌ Ｏ１
１１３１６，６１１１Ｏ
点にも特徴がある。すなわち、１個のターゲットから−
定重さの膜を多量に得るためには、そのターゲットの総
重量を大きくする必要があり、そのために、密度の増大
を図ったものである。上記２つの点から６．０ｇ／Ｃｍ
以上の密度を有する必要があり、好ましくは６．２ｇ／
ｃｍ３以上である。Table 1: Target density and wear uniformity i density g/cd
l Firing method I Uniformity of wear lllito Pressureless sintering x 1615.2 1 # l
Δ 11815.7 1 Hot press 1 Δ 119+5.
8 Pressure Sintering 1 Δ I1101 6.
0 1 Honfu Fpu J l
o H11116,21〃l O1 11316,6111O There is also a feature in the point. That is, from one target -
In order to obtain a large amount of film with a constant weight, it is necessary to increase the total weight of the target, and therefore the density is increased. 6.0g/Cm from the above two points
It is necessary to have a density of at least 6.2 g/
cm3 or more.
上記、高密度のターゲットはホットプレスを適用するこ
とによって好適に製造される。処理中、生成ＷＯ□の還
元を防止するために、モールドとして酸化物系又は窒化
物系セラミックス或いはこれらの複合材を用いる。The above-mentioned high-density target is suitably manufactured by applying hot pressing. During the treatment, oxide-based or nitride-based ceramics or a composite material thereof is used as a mold in order to prevent reduction of the generated WO□.
また、ＷＯＩ は高温において容易に酸素と分離し、還
元され易いため、ホットプレス中には酸素を充分に供給
できるようにする必要があり、具体的には、高圧の酸素
又は空気をモールド周辺に送る等の手段によって、酸素
を強制的に供給する方法、あるいは空気の循環を充分に
行う方法のいずれでもよい。In addition, since WOI easily separates from oxygen and is easily reduced at high temperatures, it is necessary to supply sufficient oxygen during hot pressing. Specifically, high-pressure oxygen or air must be supplied around the mold. Either a method of forcibly supplying oxygen by means such as a method of supplying oxygen, or a method of sufficiently circulating air may be used.
ホットプレスは９００−１０００℃の温度範囲で行い、
その時の保持圧力は１００ｋｇ／ ｃｄ以上とする。Hot pressing is performed at a temperature range of 900-1000℃,
The holding pressure at that time shall be 100 kg/cd or more.
しかしながら、上記温度での保持が長すぎると結晶粒の
成長による割れを生じたり、ＷＯ□の還元が進むことも
あり、保持時間としては２時間以内とするのが好ましい
。この場合の加熱は高周波誘導加熱によるが、発熱体と
しては、モールドを内包できる耐熱性の導電体を用いる
。However, if the temperature is kept at the above temperature for too long, cracks may occur due to the growth of crystal grains, and reduction of WO□ may proceed, so the holding time is preferably within 2 hours. Heating in this case is performed by high-frequency induction heating, and the heating element is a heat-resistant conductor capable of enclosing the mold.
この方法では大型成形体が容易に得られ、しかも成形体
は容易に切断、切削ができ、所定の寸法に加工すること
により、スパッタリング用又は電子ビーム蒸着用ターゲ
ットとする。In this method, a large molded body can be easily obtained, and the molded body can be easily cut and cut, and by processing it into a predetermined size, it can be used as a target for sputtering or electron beam evaporation.
実施例１
第１図に示すホットプレス装置を用いて、以下のように
して焼結体を得た。Example 1 A sintered body was obtained in the following manner using the hot press apparatus shown in FIG.
すなわち、ＷＯ，の粉末を充填した内径が８０ｍのアル
ミナ製モールドｌをステンレススティールからなる発熱
体２の中に置き、大気中で加熱した。That is, an alumina mold 1 with an inner diameter of 80 m filled with WO powder was placed in a heating element 2 made of stainless steel and heated in the atmosphere.
酸素の供給が充分行われるように、発熱体下部および保
護管３下部に空隙を設け、空気が充分に流通するように
した。加熱保持は９５０℃で１時間とし、１４０ｋｇ／
ｃｊのプレス圧力を維持した。In order to ensure a sufficient supply of oxygen, gaps were provided at the bottom of the heating element and at the bottom of the protective tube 3 to allow sufficient air circulation. Heating was held at 950℃ for 1 hour, and 140kg/
The press pressure of cj was maintained.
こうして得られた焼成体の密度は６．７８／ｃ＋ｍであ
った。これをサンプルｌとした。The density of the fired body thus obtained was 6.78/c+m. This was designated as sample 1.
比較のため、以下の手順で常圧焼結により焼結体を得た
。For comparison, a sintered body was obtained by pressureless sintering according to the following procedure.
すなわち、サンプルｌと同一のＷ Ｏｓ の粉末にバイ
ンダーとして七チルを１．５重量％添加し、メタノール
で充分に湿式混合した後乾燥して出発原料を得た。これ
を冷間プレスによりφ９０■ｘ８１Ｉｌｔの成形体とし
、３００℃で１時間脱脂処理した後、１０５０℃で１時
間、大気雰囲気中で常圧焼成した。That is, 1.5% by weight of heptyl was added as a binder to the same W Os powder as in sample 1, and the mixture was thoroughly wet-mixed with methanol and then dried to obtain a starting material. This was cold pressed into a molded body of φ90×81 Ilt, degreased at 300° C. for 1 hour, and then fired at normal pressure at 1050° C. for 1 hour in the air atmosphere.
これをサンプル２とした。This was designated as sample 2.
さらに、サンプルｌとサンプル２をφ８０ｍｍｘ６ＩＩ
ＩＩＩＩｔのスパッタリング用ターゲットに仕上加工し
た。Furthermore, sample 1 and sample 2 are made into φ80mm x 6II
It was finished into a IIIt sputtering target.
上記により製作した２個のターゲットをＣｕ製パッキン
グプレートに各々接合後、同一条件でスパッタリングを
実施した。After each of the two targets manufactured as described above was bonded to a Cu packing plate, sputtering was performed under the same conditions.
基板にはガラス板を用い、スパッタ条件は下記の通りで
ある。A glass plate was used as the substrate, and the sputtering conditions were as follows.
スパッタ方法：ＲＦマグネトロンスパッタ負荷電力
： １５０Ｗ
Ａｒ圧力 ： ６ ｘｌＯ−Ｔｏｒｒスパッタリング
実験の結果は東２図に示すように、密度の低い従来のタ
ーゲットに比較して、本発明による高密度のターゲット
はスパッタリングによる消耗量が大幅に低減された。Sputtering method: RF magnetron sputtering load power
: 150W Ar pressure: 6xlO-Torr The results of the sputtering experiment are shown in Figure 2. Compared to the conventional target with low density, the high-density target according to the present invention has significantly reduced consumption due to sputtering. Ta.
本発明のターゲットの効果を挙げると以下の通りである
。The effects of the target of the present invention are as follows.
イ、消耗されるターゲットの厚さは大幅に低減できる。B. The thickness of the target that is consumed can be significantly reduced.
口、消耗面は均一となり、局所的な消耗がないため、タ
ーゲットの寿命が大幅に長くなる。The mouth, the wear surface is uniform, and there is no local wear, so the life of the target is significantly extended.
第１図は本発明のターゲットを焼結するための装置の例
を示す図、第２図はターゲット密度と消耗状態の関係を
示す図である。
１：アルミナ製モールド
２：発熱管 ３：保護管
第１図
第２図
て ［＼FIG. 1 is a diagram showing an example of an apparatus for sintering a target of the present invention, and FIG. 2 is a diagram showing the relationship between target density and consumption state. 1: Alumina mold 2: Heat generating tube 3: Protection tube Figure 1 Figure 2
Claims (3)
なり、密度が６．０ｇ／ｃｍ＾３以上の成形体よりなる
ことを特徴とするターゲット。1. A target comprising a molded body having a uniform composition of WO_x (X = 2.0 to 3.0) and a density of 6.0 g/cm^3 or more.
充填し、酸素供給雰囲気中でホットプレスを行うことを
特徴とするターゲットの製造方法。2. A method for manufacturing a target, which comprises filling a ceramic mold with WO_3 powder and hot pressing in an oxygen supply atmosphere.
クスとＳｉＣまたはＳｉ＿３、Ｎ＿４ウィスカーの複合
材からなることを特徴とする請求項２記載のターゲット
の製造方法。3. 3. The method for manufacturing a target according to claim 2, wherein the mold is made of a composite material of ceramics such as oxides, nitrides, and carbides and SiC or Si_3 and N_4 whiskers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1288524A JP2693599B2 (en) | 1989-11-06 | 1989-11-06 | Target and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1288524A JP2693599B2 (en) | 1989-11-06 | 1989-11-06 | Target and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03150357A true JPH03150357A (en) | 1991-06-26 |
| JP2693599B2 JP2693599B2 (en) | 1997-12-24 |
Family
ID=17731354
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1288524A Expired - Lifetime JP2693599B2 (en) | 1989-11-06 | 1989-11-06 | Target and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2693599B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013039251A1 (en) * | 2011-09-15 | 2013-03-21 | 三菱マテリアル株式会社 | Sputtering target and method for producing same |
| CN110357626A (en) * | 2019-07-26 | 2019-10-22 | 中国建筑材料科学研究总院有限公司 | Doped tungsten oxide target and preparation method thereof |
| WO2020189428A1 (en) * | 2019-03-15 | 2020-09-24 | 三菱マテリアル株式会社 | Tungsten oxide sputtering target |
| WO2020189480A1 (en) * | 2019-03-15 | 2020-09-24 | 三菱マテリアル株式会社 | Tungsten oxide sputtering target |
| CN113423859A (en) * | 2019-03-15 | 2021-09-21 | 三菱综合材料株式会社 | Tungsten oxide sputtering target |
| KR20220036347A (en) | 2020-09-15 | 2022-03-22 | 제이엑스금속주식회사 | Cu-W-O CuW-O SPUTTERING TARGET AND OXIDE THIN FILM |
| KR20220122465A (en) | 2021-02-26 | 2022-09-02 | 제이엑스금속주식회사 | Oxide sputtering target and production method thereof, and oxide thin film |
-
1989
- 1989-11-06 JP JP1288524A patent/JP2693599B2/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013039251A1 (en) * | 2011-09-15 | 2013-03-21 | 三菱マテリアル株式会社 | Sputtering target and method for producing same |
| JP2013076163A (en) * | 2011-09-15 | 2013-04-25 | Mitsubishi Materials Corp | Sputtering target and method for manufacturing the same |
| WO2020189428A1 (en) * | 2019-03-15 | 2020-09-24 | 三菱マテリアル株式会社 | Tungsten oxide sputtering target |
| WO2020189480A1 (en) * | 2019-03-15 | 2020-09-24 | 三菱マテリアル株式会社 | Tungsten oxide sputtering target |
| CN113423859A (en) * | 2019-03-15 | 2021-09-21 | 三菱综合材料株式会社 | Tungsten oxide sputtering target |
| CN110357626A (en) * | 2019-07-26 | 2019-10-22 | 中国建筑材料科学研究总院有限公司 | Doped tungsten oxide target and preparation method thereof |
| KR20220036347A (en) | 2020-09-15 | 2022-03-22 | 제이엑스금속주식회사 | Cu-W-O CuW-O SPUTTERING TARGET AND OXIDE THIN FILM |
| KR20220122465A (en) | 2021-02-26 | 2022-09-02 | 제이엑스금속주식회사 | Oxide sputtering target and production method thereof, and oxide thin film |
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| Publication number | Publication date |
|---|---|
| JP2693599B2 (en) | 1997-12-24 |
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