TWI385138B - Ceramic components and corrosion resistance components - Google Patents
Ceramic components and corrosion resistance components Download PDFInfo
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- TWI385138B TWI385138B TW097101802A TW97101802A TWI385138B TW I385138 B TWI385138 B TW I385138B TW 097101802 A TW097101802 A TW 097101802A TW 97101802 A TW97101802 A TW 97101802A TW I385138 B TWI385138 B TW I385138B
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- 239000000919 ceramic Substances 0.000 title claims description 78
- 238000005260 corrosion Methods 0.000 title claims description 8
- 230000007797 corrosion Effects 0.000 title claims description 8
- 239000002245 particle Substances 0.000 claims description 96
- 238000010304 firing Methods 0.000 claims description 27
- 238000007088 Archimedes method Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 28
- 239000011148 porous material Substances 0.000 description 24
- 238000000034 method Methods 0.000 description 14
- 238000005530 etching Methods 0.000 description 12
- 239000010419 fine particle Substances 0.000 description 12
- 238000000465 moulding Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- 150000001639 boron compounds Chemical class 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 229910052810 boron oxide Inorganic materials 0.000 description 5
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 5
- 230000003628 erosive effect Effects 0.000 description 5
- 230000002159 abnormal effect Effects 0.000 description 4
- 238000000635 electron micrograph Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 208000037584 hereditary sensory and autonomic neuropathy Diseases 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- -1 lithium fluoride Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- RIKSBPAXKLQKOR-UHFFFAOYSA-M [O-2].O[Ta+4].[O-2] Chemical compound [O-2].O[Ta+4].[O-2] RIKSBPAXKLQKOR-UHFFFAOYSA-M 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000003112 potassium compounds Chemical class 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Description
本發明之形態一般係有關用於處理被處理基板之處理裝置的耐腐蝕性構件，具良好的耐電漿性特性、且具良好的耐微粒特性之陶瓷構件。
半導體或液晶製造裝置用之室內構件係於電漿處理裝置內導入氟系、氯系氣體，求取高度耐電漿性之材料。作為具有良好耐電漿性材料者被揭示極多高純度氧化鋁等之高純度陶瓷材料。近年來倍受矚目的有三氧化二釔極具良好的耐電漿性。又，進行蝕刻時，伴隨構件之侵蝕而產生灰塵，該灰塵附著於處理基板而出現微粒污染之不適狀。因此，被揭示具有高度電漿性，同時由微細粒子所成之構件，揭示粒界侵蝕少，雜質量少之材料。
一般公知者，陶瓷於其燒成步驟務必以高溫進行，伴隨粒子成長之燒結，故較啟始原料之粒徑大。以大粒子所構成之陶瓷，公知者為較易產生脫落。
又，電漿所曝露部份出現氣孔時，則將成電漿侵蝕之源點，導致耐電漿性不良乃公知者。
作為電漿構件之先行技術有縮小粒徑後不易脫粒者，含於燒結體中之氣孔率變小之方法。三氧化二釔為不易燒結材料，因此為取得堅固的燒結體務必於高溫下燒成。為此，促進粒子成長，無法取得以小粒徑所構成之燒結體。
如：特開2006-21990號公報中被揭示有使用平均粒徑0.7μm之原料粉末，以1700℃進行燒成時，取得平均粒徑4μm，容積密度4.90g/m3
之三氧化二釔燒結體。
更於特開2005-8482號公報中被揭示有使用平均粒徑1.2μm之原料粉末，於1650℃下進行燒成時，取得平均粒徑2μm，容積密度4.64g/m3
之三氧化二釔燒結體，於1710℃下進行燒成時，取得平均粒徑12μm，容積密度4.90g/m3
之三氧化二釔燒結體。由此證明，以一般的燒成方法下製作堅固之三氧化二釔燒結體時，務必於1700℃以上之溫度下進行燒成。
本發明形態係提供一種抑制陶瓷構件中之異常粒成長，減少氣孔產生，同時由小粒子所構成下，不易出現脫粒，具良好的耐電漿性之陶瓷構件。
為達成該目的，本發明之一實施形態中，以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，可作成其構成該陶瓷構件之粒子的平均粒徑為未達1.5μm，且藉由阿基米德法所測定取得之開氣孔率為未達0.5%者為其特徵之陶瓷構件。
本發明之其他實施形態中，以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，可作成其構成該陶瓷構件之粒子最大粒徑為未達3μm，且藉由阿基米德法所測定取得之開氣孔率為未達0.5%者為其特徵之陶瓷構件。
更理想之形態中，以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，可作成含Y3
BO6
於該陶瓷構件中之陶瓷構件。
本發明理想形態中，以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，可作成該陶瓷構件之厚度為0.3mm以上之陶瓷構件。
又，本發明之耐腐蝕性構件係可作成使本發明之一實施形態中之陶瓷構件配設於務必耐腐蝕性之部位所成之耐腐蝕性構件。
本發明之形態係可提供一種，減少開氣孔後，可減少成為電漿侵蝕源點之個處，而具有良好的耐電漿性之陶瓷構件。而以抑制異常粒子成長之小粒子所構成後，可降低因發塵造成之微粒污染。
以下進行本件所使用語句之說明。
本發明之陶瓷構件係指藉由三氧化二釔粉末之燒成所取得之陶瓷構件，陶瓷構件表面不管其硬化面、研磨、磨削面等。以三氧化二釔為主成份係指構成陶瓷構件之金屬元素中之釔元素佔主要部份之意。其中，釔元素佔構成陶瓷構件之金屬元素之主要部份係指作為釔元素於陶瓷構件
中之含量者，對於構成陶瓷構件之所有金屬元素量而言，一為50重量%以上者宜，較佳者為93重量%以上，更佳者為95重量%以上。
本發明之粒徑係指1個個構成陶瓷構件之固體結晶粒子之大小，陶瓷構件中，相互於粒子界面分段之各個粒子之大小。
本發明之平均粒徑係指藉由測面米制所算出之值。平均粒徑之測定係使試料進行鏡面研磨後，於大氣氛圍中進行熱蝕刻，利用藉由SEM之觀察像，依測面米制法算出平均粒徑。
本發明之平均粒徑之測定係利用Jeffries之測面米制法進行者。
(參考文獻：Z.Jeffries ,Chem. Met. Engrs., 16 ,503-504 (1917); ibid., 18, 185 (1918))。
將任意2~3個熱蝕刻之試料以10000倍進行SEM拍攝，於照片上描繪面積(A)之已知之圓，藉由下式由圓內之粒子數nC
與圓周之粒子數ni
求出每單位面積之粒子數NG
。
NG
=(nC
+1/2ni
)/(A/100002
)
1/NG
為1個粒子所佔面積。由此利用下式算出相當圓粒徑(D)作為平均粒徑。
D=2/(π NG
)1/2
本發明之熱蝕刻係使試料進行鏡面研磨後，對於燒成溫度而言，以昇溫速度300℃/h進行昇溫至300~400℃之低溫，保持10~30分鐘後進行爐內放冷之步驟。藉由此熱處理，使1個個粒子進行熱膨脹，經由冷卻收縮時粒子界面出現凹陷。藉由此，可觀測粒子之大小。
本發明之最大粒徑係指使施予熱蝕刻之試料，以10000倍之SEM觀察下進行拍攝，藉由所觀察之最大粒子之單向最大粒徑(Krumbein徑)取得之大小。
本發明之阿基米德法係指JIS規格(JIS R1634)所示之密度測定方法。水合方法係利用真空法、媒液中使用蒸餾水進行測定。開氣孔係指存在於試料表面之氣孔。開氣孔係可以阿基米德法進行測定，以開氣孔率示之。所測定之開氣孔率當以試料之外形容積為1時，其中所佔開氣孔部份之容積的百分比。
本發明之原料粉末粒徑之表記所使用之比表面積係藉由JIS規格(JIS R1626)所示之BET法者。
公知者於提昇耐電漿性時，務必減少氣孔之存在。一般公知者有於HIP處理下減少氣孔之處理，惟卻不易去除存在於堅固化結束之燒結體中之數μm以上之粗大氣孔。因此，於燒結時務必減少氣孔。
一般，氣孔大小約所構成燒結體粒徑之1/10。又，公知者構成燒結體極之粒徑與氣孔之平均粒徑及氣孔之體積為如下關係式。
D=d/f
D：構成粒子極限粒徑
d：氣孔之平均徑
f：氣孔之體積
為減少氣孔之體積，務必縮小氣孔之大小。因此，務必縮小所構成燒結體粒子後，同時抑制異常粒子成長，由均質粒子所構成。惟，粒子成長於燒結過程中，為去除氣孔促進堅固化為不可或缺者，務必有某種程度之粒子成長。
本發明之一實施形態中發現至少滿足，理想之平均粒徑為未達1.5μm、最大粒徑為未達3μm之1個條件時，將具有經由燒結體中之氣孔的抑制效果。
由耐微粒特性之觀點視之，被期待更縮小平均粒徑與
最大粒徑，而由易於製作堅固之陶瓷構件之觀點視之，其平均粒徑與最大粒徑為0.1μm以上者宜。構成陶瓷構件之粒小的移動係依存溫度，同時亦依存促進燒結之溫度。本發明之一實施形態中發現，具充足之燒結與同時可達成微結構造之構成粒子尺寸範圍及可判定極限值。
本發明之一實施形態中，以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，依阿基米德法所測定取得之開氣孔率為未達0.5%，較佳者為0.3%以下之陶瓷構件後，可提昇耐電漿性、耐微粒特性。另外，理論上，開氣孔率為0%為更佳。因此，開氣孔率為0%以上者宜。
本發明之一實施形態中，以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，構成該陶瓷構件之粒子平均粒徑為未達1.5μm，較佳為1μm以下，且依阿基米德法所測定取得之開氣孔率為未達0.5%，較佳者為0.3%以下為其特徵因此可取得由堅固之氣孔少的微細粒子所成之陶瓷構件。另外，由易於製作堅固材質之陶瓷構件之觀點視之，其平均粒徑為0.1μm以上者更佳。又，理論上，開氣孔率為0%者更佳。因此，開氣孔率為0%以上者宜。
本發明之一實施形態中，以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，構成該陶瓷構件之粒子的最大粒徑為未達3μm、較佳者為1.5μm以下，且依阿基米德法所測定取得之開氣孔率為未達0.5%，較佳者為0.3%以下者為其特徵因此可取得由堅固之氣孔少的微細粒子所成之陶瓷構件。另外，由易於製作堅固之陶瓷構件之觀點視之
，其平均粒徑為0.1μm以上更佳。又，理論上，開氣孔率為0%者更佳。因此，開氣孔率為0%以上者宜。
以三氧化二釔為主成份，藉由燒成取得之陶瓷構件中，其陶瓷構件之厚度更為0.3mm以上者宜。更佳者為1mm以上。使陶瓷構件增厚時，可長期於腐蝕環境下使用。由易於製作之觀點視之，其陶瓷構件之厚度為10cm以下者宜。此所謂厚度係指由至少曝露於電漿氛圍或腐蝕環境下之陶瓷構件之表面之深度方向。
陶瓷構件之形狀如：板狀、薄片狀、棒狀、球狀、圓筒狀、梯形狀、圓柱狀、中空狀、稜形狀等例。此等為相互組合之複雜形狀者亦無妨。另外，陶瓷構件之表面形狀亦可為平滑狀或凹凸形狀者。
本發明之理想形態中，使三氧化二釔粉末成形，於1200~1600℃，較佳者1400~1550℃，更佳者1400~1500℃下進行燒成，必要時進行磨削、研磨加工。於此溫度下燒成後，抑制粒子成長，可取得由微細粒子所成之陶瓷構件。
更理想者，對於三氧化二釔，於該溫度下進行添加生成液相之助劑。藉由添加燒結助劑後，可提高燒結性，更可易於該溫度下之燒成。
作為該助劑例者如：可適於使用氧化硼、硼酸等之硼化合物，氟化鋰等之鋰化合物、氟化鉀等之鉀化合物等。最佳者為添加硼化合物。
原料之混合方法可利用用於如球磨器之陶瓷製造步驟中之一般常法。三氧化二釔原料粉末之粒徑並未受限，平均10μm以下者宜，更佳者為2μm以下。下限值雖未限定，而恐降低成形性，因此為亞微型者宜。伴隨如球磨器之粉碎步驟之混合方法不僅可使粒徑變細，亦具粉碎粗大粒子之效果，可取得均質、微細粒子所成之陶瓷構件為理想者。
本發明實施形態中成形方法可藉由使造粒之粉末進行加壓成形、CIP等之乾式成形方法取得成形體。成形並未受於乾式成形，可利用擠壓成形、射出成形、薄片成形、鑄入成形、凝膠鑄塑成形等成形方法取得成形體。乾式成形時，可利用加入黏合劑，利用噴霧乾燥等，作成顆粒。
本發明實施形態中，燒成可於大氣氛圍下，進行未達1600℃之燒成，可於具有SiC發熱體、耐熱發熱體之電爐下之燒成。燒成未受限於大氣氛圍中，亦可於氮、氬等不活性氛圍中、真空中之燒成。燒成時間可於0.5~8小時之間選取之。燒成溫度可於1200~1600℃之範圍下進行選取，為1400~1550℃者宜，更佳者為1400~1500℃之燒成。於此溫度下進行燒成後，抑制粒子成長，可取得微細粒子
所成之陶瓷構件。
為提高燒結性，於陶瓷構件中置入硼化合物時，則於燒成中易使硼化合物蒸散，故施予隔焰等進行燒成者宜。硼化合物於燒成之過程中形成Y3
BO6
，於1100~1600℃之溫度下形成液相，促進燒成。此Y3
BO6
之液相的生成於低溫之燒成係抑制陶瓷粒子之粒子成長，可取得由微細粒子所構成之陶瓷構件。
取得之燒結體可進行燒成溫度以下之溫度範圍下之HIP處理。藉由此，開氣孔率為未達0.1%，更佳者為未達0.05%，可取得接近理論密度之堅固材質燒結體。
作為生成該Y3
BO6
結晶之硼化合物者並未限於氧化硼、可使用硼酸、氮化硼、碳化硼、YBO3
、Y3
BO6
等之硼化合物，其中又以氧化硼、硼酸、YBO3
為適用者。
取得之陶瓷構件係進行鏡面研磨，對於燒成溫度，以昇溫速度300℃/h下進行昇溫至300~400℃之低溫，保持10~30分鐘進行熱蝕刻。取得之試料可利用SEM進行觀測粒子形狀。
本發明之一實施形態所取得之陶瓷構件可適用於真空室、玻璃鐘罩、受容器、壓緊環、焦距環、橡皮絕緣環、切邊環、絕緣環、襯墊、模擬晶片，為產生高周波電漿之管，為產生高周波電漿之圓筒，為支撐半導體晶圓之升降針、噴淋板、緩衝板、波紋管蓋、上部電極、下部電極、室內部之構件固定用之螺絲、螺絲間隙、自動搖控杆等電漿氛圍中所曝露之半導體或液晶製造裝置用構件。如真空
室、玻璃鏡罩被利用於進行電漿照射之內壁面，焦距環、橡皮絕緣環可利用於電漿氛圍所連接之面。另外，其他構件亦可利用於電漿氛圍所曝露之面。
本發明之一實施形態之陶瓷構件更因具有1014
Ω‧cm以上之體積電阻，故可利用於半導體晶圓、石英晶圓中進行微細加工之蝕刻裝置等之靜電夾頭。
又，本發明之一實施形態之陶瓷構件可利用於為搬運氟化氫等之腐蝕溶液、腐蝕氣等之搬運管等之抗腐蝕用構件，使用腐蝕溶液進行化學處理等時所使用之坩堝等。
準備原料之三氧化二釔粉末(比表面積11~15g/m3
)與氧化硼(試藥級)，使氧化硼添加量為0~8wt%，加入分散劑‧黏合劑‧脫模劑，藉由球磨器進行粉碎攪拌混合。混合後，藉由噴霧乾燥器進行造粒。取得造粒粉末進行加壓成形後，進行CIP成形。藉由噴霧乾燥器之造粒與藉由CIP處理，可取得提昇成形體密度與安定之燒成體。所得成形體進行脫脂後，於大氣氛圍中，1400℃~1500℃下進行燒成。表1係代表所得燒結體與平均粒徑，最大粒徑及開氣孔率之關係。
實施例1~5係變更硼添加量後，進行試驗之結果。燒結體之平均粒徑為0.2~1.5μm之範圍，由極微細之粒子所構成。最大粒徑更為3μm以下，具有微細且狹窄之粒度分佈之燒結體。由此顯示開氣孔率為0.24%以下之低值。
比較例1係於1600℃下，燒成硼無添加試料之結果。平均粒徑為0.35μm之極細小粒徑所構成。惟開氣孔率具有0.76%之極多氣孔。此其最大粒徑為0.8μm之極小粒徑。
比較例2係添加8wt%之硼添加量之系。比較例2中被證明為異常成長之粒子，為大粒子者由超出3μm之粒子所構成。於前述實施例中被確定某種程度之粒子成長務必進行燒結，而過剩之粒子成長被證明有阻礙燒結之傾向
。因此，顯示高達24%之高值的多氣孔之開氣孔率。
比較例3係代表使用比表面積35~45m2
/g之原料粉末時。於1400℃之大氣氛圍中進行燒成取得之燒結體被確定為容積密度3.87g/m3
與稍有未堅固(consolidation)化者，而其構成粒子之平均粒徑為0.26μm與出現狀似無粒子成長狀態。但是，最大粒徑為0.7μm程度，使燒結愈充分達成則粒子愈無法成長。因此並非成為充分的堅固體。
由以上結果證明，平均粒徑為0.2~1.5μm與微細粒子所構成，同時出現燒結體中所存在之異常粒成長之粒子未達3μm者，具有抑制作為電漿侵蝕起點之開氣孔的存在之效果，具有耐電漿性之效果。而由於微細粒子所構成者，故亦具有耐微粒性。
為評定本發明之一實施形態之陶瓷構件之耐電漿性，而使實施例4及比較例1利用離子反應蝕刻裝置(Anelva股份公司DEA-506)，蝕刻氣體係以CF4
(40sccm)+O2
(10sccm)，進行1000W、30小時之電漿照射處理，其結果示於圖1~4。實施品相較於比較例，證明電漿照射後仍呈現極為良好之表面形狀。
[圖1]代表藉由本發明之一實施例顯示陶瓷構件之電漿照射前之表面狀態之電子顯微鏡照片之圖。
[圖2]代表藉由本發明之一實施例顯示陶瓷構件之電漿照射前之表面狀態之電子顯微鏡照片之圖。
[圖3]代表比較例1所示之陶瓷構件之電漿照射前之表面狀態之電子顯微鏡照片之圖。
[圖4]代表比較例1所示之陶瓷構件之電漿照射前之表面狀態之電子顯微鏡照片之圖。
Claims (5)
- 一種陶瓷構件，其係釔元素在陶瓷構件中的含量相對於構成陶瓷構件的金屬元素總量而言，以氧化物換算在93重量%以上、藉由燒成取得之陶瓷構件，其特徵為構成該陶瓷構件之粒子平均粒徑為未達1.5μm，且經由阿基米德法測定取得之開氣孔率為未達0.5%。
- 一種陶瓷構件，其係釔元素在陶瓷構件中的含量相對於構成陶瓷構件的金屬元素總量而言，以氧化物換算在93重量%以上、藉由燒成取得之陶瓷構件，其特徵為構成該陶瓷構件之粒子之最大粒徑為未達3μm，且經由阿基米德法測定取得之開氣孔率為未達0.5%。
- 如申請專利範圍第1項或第2項之陶瓷構件，其中，該陶瓷構件中含Y3 BO6 。
- 如申請專利範圍第1項或第2項之陶瓷構件，其中，該陶瓷構件之厚度為0.3mm以上。
- 一種耐腐蝕性構件，其特徵係將申請專利範圍第1項至第4項中任一項之陶瓷構件配設於需要耐腐蝕性之部位所成。
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| EP (1) | EP2123615A4 (zh) |
| JP (1) | JP4197050B1 (zh) |
| KR (1) | KR20090101245A (zh) |
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| WO (1) | WO2008088071A1 (zh) |
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| JP5117891B2 (ja) * | 2008-03-11 | 2013-01-16 | 日本碍子株式会社 | 酸化イットリウム材料、半導体製造装置用部材及び酸化イットリウム材料の製造方法 |
| JP5190809B2 (ja) * | 2008-08-28 | 2013-04-24 | Ｔｏｔｏ株式会社 | 耐蝕性部材およびその製造方法 |
| US9850568B2 (en) | 2013-06-20 | 2017-12-26 | Applied Materials, Inc. | Plasma erosion resistant rare-earth oxide based thin film coatings |
| US10464849B2 (en) * | 2015-12-08 | 2019-11-05 | Edward J. A. Pope | Fast-densified ceramic matrix composite and fabrication method |
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| TWI223646B (en) * | 2001-11-26 | 2004-11-11 | Ngk Insulators Ltd | Aluminum nitride ceramics, members for use in a system for producing semiconductors, corrosion resistant members and conductive members |
| US20050281302A1 (en) * | 2003-11-25 | 2005-12-22 | Lee Hee D | YAG lasing systems and methods |
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| JP4197050B1 (ja) | 2008-12-17 |
| EP2123615A4 (en) | 2012-05-09 |
| US20080176735A1 (en) | 2008-07-24 |
| US7799719B2 (en) | 2010-09-21 |
| EP2123615A1 (en) | 2009-11-25 |
| TW200902474A (en) | 2009-01-16 |
| WO2008088071A1 (ja) | 2008-07-24 |
| JP2009173459A (ja) | 2009-08-06 |
| KR20090101245A (ko) | 2009-09-24 |
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