JP5465381B2 - 被覆した研磨材料及びその製造方法 - Google Patents
被覆した研磨材料及びその製造方法 Download PDFInfo
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- JP5465381B2 JP5465381B2 JP2007531862A JP2007531862A JP5465381B2 JP 5465381 B2 JP5465381 B2 JP 5465381B2 JP 2007531862 A JP2007531862 A JP 2007531862A JP 2007531862 A JP2007531862 A JP 2007531862A JP 5465381 B2 JP5465381 B2 JP 5465381B2
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Description
本発明の一つの要旨に基づき、超硬質研磨粒子の被覆方法(又はコーティング方法)は、ガラス質を好む表面を有する複数の超硬質研磨粒子を供給する工程、酸化物前駆体材料を用いて超硬質研磨粒子を被覆する工程、及び被覆した超硬質研磨粒子を熱処理して被覆(コート又はコーティング)を乾燥して精製(又は純化)する工程を含む。
本発明は、のこ引き(又はソーイング)、穴あけ、ドリルあけ、掘削(又はドリリング)、研削、破砕、粉砕、研磨、ひく、磨く、とぐ(又はグラインディング)、研磨、つや出し、磨き、磨き仕上げ(又はポリッシング)及び他の研磨材料(又は研削材料)及び切断、切削、切り抜き(又はカッティング)用途に広く使用される被覆した研磨粒子及び材料に関する。
ミクロン、サブミクロン又はナノ粒子サイズダイヤモンドの場合、例えば硝酸及び/又は硫酸の混合物等の濃い酸化力のある酸で加熱する等の方法を用いて、C−OH、C−O−C、C=O及びO=C−O−で、主に構成されるべき、表面の終点である表面官能基を、生じさせてよい。別法では、表面をHで終わらせるために、20%水素/アルゴン中900℃で気体熱処理し、その後20%酸素/アルゴン中約480℃で熱処理して酸素種によって占められた表面を形成してよい。ダイヤモンド表面に結合した酸素系官能基を生ずる他の方法も使用することができる。酸化したダイヤモンド表面は、ガラス質を好むようになり、即ち、特に水和酸化物(又はハイドレーテッドオキサイド:hydrated oxide)構造を含む酸化物と化学結合を形成することができる。
模式図の2(a)部分を参照すると、前駆体水和酸化物材料を生成し所望の被覆材料にする一般的なゾルゲル技術が使用される。そのようなアプローチの一般的な例は、例えば尿素等の有機化合物の存在下、例えば100℃の温度で硫酸アルミニウム溶液を加水分解して、懸濁物中の粒子を被覆することを含む。このようにして、水和酸化アルミニウム被覆を生じさせることができる。
さて、被覆した粒子は、温度プログラム熱処理又は反応を受ける。残留揮発性不純物の除去を制御するために、密度を高め(圧縮し又は緻密にし)焼結するために、他の構造相に変えるために、及び被覆をガスと化学的に反応させて他の材料種と相にするために、選択された気体環境(条件又は雰囲気)下で、選択された加熱速度で、選択されたトップ温度に、選択された時間、このことは行われる。好ましいアプローチは、注意深く選択し制御した流速で、流通ガス系(又はシステム)を用いることである。被覆した粒子材料の加熱を、環状炉、粒子をゆっくり「攪拌」するように組織化され、溶解又は凝集を防止する回転する環状炉、又は選択した制御気体環境で粒子材料を制御加熱するための適切な炉設備で行うことができる。
以下に本発明の主な態様を記載する。
1.ガラス質を好む表面を有する複数の超硬質研磨粒子を供給する工程、酸化物前駆体材料を用いて超硬質研磨粒子を被覆する工程、及び被覆した超硬質研磨粒子を熱処理して被覆を乾燥し精製する工程を含む超硬質研磨粒子の被覆方法。
2.被覆した超硬質研磨粒子を処理して、酸化物前駆体材料を、酸化物前駆体材料の酸化物、窒化物、炭化物、酸窒化物、酸炭化物又は炭窒化物、又は酸化物前駆体材料の元素形態、又はそれらの組み合わせに変換する上記1に記載の方法。
3.酸化物前駆体材料は、非晶質又はナノ結晶性酸化物、水酸化物又はオキソ水酸化物である上記1又は2に記載の方法。
4.超硬質研磨粒子は、ダイヤモンド、立方晶窒化ホウ素、炭化ケイ素、窒化ケイ素、炭化ホウ素及び亜酸化ホウ素(B 6 O)を含んで成る群から選択される上記1〜3のいずれかに記載の方法。
5.超硬質研磨粒子は、ダイヤモンド又は立方晶窒化ホウ素又はこれらの材料の組み合わせであり、該粒子の表面をガラス質を好むようにするために該粒子を表面処理法で処理する上記1〜4のいずれかに記載の方法。
6.変換された酸化物前駆体材料は、該酸化物前駆体材料のミクロン、サブミクロン又はナノ粒子サイズ酸化物、窒化物、炭化物、酸窒化物、酸炭化物及び炭窒化物又は元素形態の該酸化物前駆体材料、又はそれらの組み合わせから選択される上記1〜5のいずれかに記載の方法。
7.変換された酸化物前駆体材料は、アルミニウム、チタン、ケイ素、バナジウム、ジルコニウム、ニオブ、ハフニウム、タンタル、クロム、モリブデン及びタングステンの酸化物、窒化物、炭化物、酸窒化物、酸炭化物及び炭窒化物、元素形態のモリブデン及びタングステン、及びこれらの材料の適切な組み合わせから選択される上記1〜6のいずれかに記載の方法。
8.変換された酸化物前駆体材料は、アルミニウム、チタン、ケイ素、バナジウム、ジルコニウム、ニオブ、ハフニウム、タンタル、クロム、モリブデン及びタングステン及びこれらの材料の適切な組み合わせのナノ粒子サイズの化合物である上記1〜7のいずれかに記載の方法。
9.変換された酸化物前駆体材料は、ナノ粒子サイズの元素形態のタングステン、モリブデン又はこれらの金属の組み合わせ又は合金である上記1〜7のいずれかに記載の方法。
10.いわゆるゾルゲル技術を用いて、超硬質研磨粒子に酸化物前駆体材料を被覆する上記1〜9のいずれかに記載の方法。
11.超硬質研磨粒子を液体媒体に懸濁し、適切な化学試薬を入れて、各粒子表面と結合し、粒子上に被覆を構築するコロイド体を形成する上記10に記載の方法。
12.適切な化学試薬は、少なくとも一種のアルコキサイド又はアルコキサイドのアルコール溶液である上記11に記載の方法。
13.液体媒体は、水とアルコールのアリコートである上記11又は12に記載の方法。
14.適切な化学試薬は、水とアルコールのアリコートである上記11に記載の方法。
15.液体媒体は、少なくとも一種のアルコキサイド又はアルコキサイドのアルコール溶液である上記11又は14に記載の方法。
16.アルコキサイドは、アルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウムから選択される元素のアルコキサイドである上記12又は15に記載の方法。
17.アルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウム元素のアルコキサイドから選択される、二種又はそれ以上のアルコキサイドを液体媒体に入れる上記12又は13に記載の方法。
18.液体媒体は、アルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウム元素のアルコキサイドから選択される、二種又はそれ以上のアルコキサイドのアルコール溶液を含んで成る上記14又は15に記載の方法。
19.適切な化学試薬又は液体媒体は、場合により、二種又はそれ以上のアルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウム元素を組み込む混合アルコキサイド化合物又はコンプレックスの溶液である上記11〜18のいずれかに記載の方法。
20.アルコールは、アルコキサイドと同じアルキル基を有する上記11〜19のいずれかに記載の方法。
21.酸化物前駆体材料被覆は、実質的に細孔性である上記1〜20のいずれかに記載の方法。
22.被覆した超硬質研磨粒子を、空気、真空又は不活性ガス中で温度制御加熱に付して、表面積が大きな細孔性非晶質被覆に付着した揮発物及び好ましくない化学種を除去する上記21に記載の方法。
23.被覆した超硬質研磨粒子を、更に熱処理又は焼成に付して、被覆を結晶化し、微粒子又はナノサイズ粒子酸化物セラミックを形成する上記22に記載の方法。
24.被覆した超硬質研磨粒子を更に熱処理に付して、被覆をガラス質にしてガラスを形成する上記22に記載の方法。
25.被覆した超硬質研磨粒子を、反応性ガス中で温度制御反応に付して、該被覆材料を非酸化物セラミック又はガラスに変換する上記21〜24のいずれかに記載の方法。
26.被覆をアンモニアガスと反応させることで窒化物を形成する上記25に記載の方法。
27.炭素質ガスと水素の混合物中で被覆を反応させることで、炭化物を形成する上記25又は26に記載の方法。
28.メタン又はエタンと水素との混合物中で被覆を反応させることで、炭化物を形成する上記27に記載の方法。
29.被覆した超硬質研磨粒子を、反応性ガス中で温度制御反応に付して、被覆材料を酸窒化物又は酸炭化物セラミック又はガラスに変換する上記21〜24のいずれかに記載の方法。
30.酸化物被覆は水素で還元可能であり、酸化物被覆をマイクロ又はナノ粒子サイズ元素又は金属に変換する上記22又は23に記載の方法。
31.チタン、バナジウム、ニオブ、タンタル、モリブデン及びタングステンの窒化物、又はバナジウム、ニオブ、タンタル、モリブデン及びタングステンの炭化物から選択される被覆を有するダイヤモンド又は立方晶窒化ホウ素粒子を含んで成る被覆した超硬質研磨粒子材料。
32.アナターゼ相チタニア、ルチル相チタニア、正方晶ジルコニア、単斜晶ジルコニア、イットリア又はマグネシアで安定化されたジルコニア、アルミナのアルファ相及び過渡的構造、及びバナジウム、ニオブ、タンタル、ハフニウム、モリブデン及びタングステンの酸化物から選択される被覆を有するダイヤモンド又は立方晶窒化ホウ素粒子を含んで成る被覆した超硬質研磨粒子材料。
33.シリカガラスで被覆されたダイヤモンド又は立方晶窒化ホウ素粒子を含んで成る被覆した超硬質研磨粒子材料。
34.ダイヤモンド又は立方晶窒化ホウ素は、ミクロン、サブミクロン又はナノサイズである上記30〜32のいずれかに記載の被覆した超硬質研磨粒子材料。
35.チタン、バナジウム、ニオブ、タンタル、アルミニウム、ケイ素、モリブデン及びタングステンの酸化物、又はチタン、バナジウム、ニオブ、タンタル及びモリブデンの窒化物又は炭化物、又はモリブデン又はタングステン金属で被覆されたミクロン、サブミクロン又はナノサイズのダイヤモンド又は立方晶窒化ホウ素粒子を含んで成る被覆した超硬質研磨粒子材料。
36.被覆の厚さは、2ミクロンより薄い上記30〜34のいずれかに記載の被覆した超硬質研磨粒子材料。
37.本発明の説明に役立つ例のいずれかを参照して実質的に本明細書で説明した上記1に記載の方法。
38.本発明の説明に役立つ例のいずれかを参照して実質的に本明細書で説明した上記1に記載の被覆した超硬質研磨材料。
50gのサブミクロン立方晶窒化ホウ素(平均粒子サイズは0.7ミクロン、大まかな(又は全般的な)サイズ範囲は0.5〜1.0ミクロン)を、硝酸カリウムを加えた発煙濃硫酸で処理した。洗浄し乾燥後、サブミクロンcBNを更に空気中600℃で30分間加熱した。これらの手順によって、cBN表面化学は酸素関連官能基によって占められ、従ってガラス質を好むことが確保された。
平均粒子サイズ2ミクロンの30gのcBN粉末を、水中15%過酸化水素、H2O2、と15%水酸化アンモニウム、NH4OHの1対1混合溶液中に懸濁させた。これは、cBN粒子表面の加水分解に役立ち、従って、ガラス質を好むようにした。その後、2ミクロンcBN粉末を、懸濁物から濾過で取り出し、脱イオン水で洗浄した。
105gの120/140USメッシュ(105〜125μm)、カットされた結晶性cBNを、沸騰32体積%塩酸で処理し、水で洗浄し、乾燥した。その後、この材料を空気中で1時間650℃で加熱し、粒子表面をわずかに酸化した。
粉砕し、分類手順によって合成ダイヤモンドソースから誘導された50gのダイヤモンドミクロン(平均粒子サイズ1.0ミクロン、大まかなサイズ範囲0.75〜1.5ミクロン)を、硝酸カリウムを加えた発煙濃硫酸で処理した。この清浄化で、ダイヤモンドが金属及び無機表面汚染物質を含まないことを確保した。その後、ダイヤモンドを、アルゴンガス流中20%酸素気流中で、480℃で1時間加熱した。この手順は、ダイヤモンド表面に付された酸素含有官能基を最大にし、表面をガラス質を好むようにした。
例4に詳述した手順を行って、約1μm平均サイズの合成ダイヤモンドに関して、結晶性アナターゼ被覆ダイヤモンド粉末を製造することができる。もし、この粉末を、流通するアルゴン中10%メタンとアルゴン中10%水素のガス混合物に、メタンと水素との適切な比で(1:4と予想される)、約1350℃の温度で数時間(好ましくは5時間より長く)暴露すると、チタニア被覆は炭化チタンに変換されることが期待された。従って、窒化チタン被覆1μmダイヤモンドが生産される。
105〜125μmの平均粒子サイズのカットされた合成ダイヤモンド20g試料を、純度が99%より高い1.25リットルのエチルアルコールに懸濁した。主に酸素含有官能基を有する表面を得るために、アルゴン中20%酸素の流通気流中で10分間480℃で、ダイヤモンド試料を予め加熱した。この激しく攪拌した懸濁物に、250mlの脱イオン水と30mlの25体積%の水酸化アンモニウム水溶液を加えた。
既知の粉砕し、分類手順によって製造された複数の0.75〜1.5ミクロンサイズのダイヤモンド粒子を、硝酸カリウムを加えた発煙濃硫酸で処理した。この手順で、ダイヤモンド表面化学が酸素関連官能基で支配され、従って、ガラス質を好むことを確保し、それによってその表面化学種がゾルゲル反応に関与することを可能とした。このダイヤモンド20gを99%純度エチルアルコール2.5リットルに超音波プローブの助けをかりて分散させ、それに、500mlの脱イオン水と60mlの25体積%水酸化アンモニウム水溶液を加えた。懸濁物をパドル攪拌機を用いて激しく攪拌し、室温(25℃)で保持した。80gのシリコンテトラエトキシシリケート[Si(OC2H5)4]の溶液を、99%純度エタノール100mlに溶かした。この溶液を12時間かけてゆっくり懸濁物に加えた。その後、攪拌を更にもう1時間続けた。その後、例6に記載したように、複数の被覆したダイヤモンド粒子を懸濁物から取り出し、洗浄し、乾燥した。
20gの十分にカットした高結晶性105〜125ミクロン直径cBN粗粒子を、沸騰32体積%塩酸中で処理し、水で洗浄し乾燥した。この材料を、激しく攪拌しながら1.8リットルの99%純エタノール、350mlの脱イオン水及び40mlの25体積%の水酸化アンモニウム水溶液の混合物に懸濁した。その後、テトラエトキシシラン[Si(OC2H5)4]の30重量%純エタノール溶液をゆっくり連続的に10時間かけて攪拌した懸濁物に加えた。攪拌をもう1時間続けた。材料を静置し、上澄み液を除去し、被覆したcBN粒子を純乾燥エタノールで洗浄した。その後、被覆した材料を真空オーブン中60℃で24時間乾燥した。その後、この被覆した材料を乾燥純アルゴン中で1分当たり3℃で800℃の温度まで加熱し、この温度で3時間保持した。その後のSEM観察で、粒子は、大部分滑らかで特徴のない外観の亀裂のないシリカ被覆で完全にカバーされた。
0.75〜1.5ミクロンダイヤモンドに対する例7に記載した被覆手順を平均サイズ1.25ミクロンのcBNミクロン粉末を被覆するために適用した。真空で60℃で24時間乾燥後のゾルゲル被覆微粉末を、アルゴン中800℃で3時間熱処理した。SEM観察の際、緻密なシリカ被覆による完全な被覆が、各個々のcBN粒子について達成されたことが示された。
110gの120/140USメッシュ(105〜125μm)、カットされた結晶性cBNを、沸騰32体積%塩酸で処理し、水で洗浄し、乾燥した。その後、この材料を空気中で1時間650℃で加熱し、粒子表面をわずかに酸化した。
0.5〜1ミクロンのおおよその粒子サイズ(0.7ミクロンの平均粒子サイズ)を有するサブミクロン立方晶窒化ホウ素を例1で記載したように酸処理した。34.0gの酸処理cBN粉末を、2020mlの純エタノールと42mlの脱イオン水に懸濁した。このcBN懸濁物を20分間超音波プローブで処理し、粒子凝集物を破壊し、その後、パドル型攪拌機で激しく機械的に攪拌した。
0.5〜1ミクロンの粒子サイズ範囲(0.7ミクロンの平均粒子サイズ)を有するサブミクロン立方晶窒化ホウ素を例1で記載したように酸処理した。25gのこの粉末を、1.5リットルの純エタノールと30mlの脱イオン水に懸濁し、25分間超音波処理をした。別のビーカーで、50mlの純エタノールに0.48gの硝酸イットリウム6水和物、Y(MO3)3・6H2Oを溶かし、その後、13.9gのジルコニウム(IV)n−プロポキサイド、化学式Zr[O(CH2)2CH3]4と追加の50mlの純エタノールを加えた。後者のビーカーの内容物をガラス棒で攪拌し、更に分離ロートで内容物を振り混ぜた。硝酸イットリウム6水和物−ジルコニウム(IV)n−プロポキサイド溶液混合物を、室温で2時間かけて滴下して攪拌したcBN懸濁物に加えた。この添加後、溶液を更に1時間10分機械的に攪拌した。その後、溶液を室温で一夜間熟成した。得られた複数の被覆された粒子は、一夜の熟成後、大いに粘性のゲルを形成したことが見出された。合計で48時間の熟成時間後、ゾルゲルを、70〜80℃の間の温度で、400mbarの減圧下、ロータリーエバポレーターで乾燥した。
12gの120/140USメッシュ(105〜125μm)、カットされた結晶性cBNを、空気中650℃で加熱し、粒子表面を酸化した。その後、この材料を攪拌し、22mlの脱イオン水を加えた200mlの純イソプロパノールに懸濁した。懸濁物を加熱し、還流下50℃に保った。
おおまかな粒子サイズ範囲0.75〜1.5ミクロンを有する1ミクロン合成ダイヤモンド粉末を、例4に記載したように酸で清浄にした。20gのこのダイヤモンド粉末を258mlの純イソプロパノールと175mlの脱イオン水を含んで成る溶液に懸濁した。還流装置でこの懸濁物を60℃に加熱し、パドル型攪拌機を用いて100rpmで機械的に攪拌した。化学式AlO3C12H27を有する24gのアルミニウムsec−ブトキサイドを100ml無水イソプロパノールに溶かし、加熱し攪拌したダイヤモンド懸濁物に1時間45分かけて滴下して加えた。アルコキサイドの添加後、懸濁物を60℃で1時間15分間攪拌を続けた。その後、約1mlの塩酸(32%)を加熱した懸濁物に加え、その後、80℃に加熱し、その温度を保ちながら更に1時間攪拌した。その後、懸濁物を室温に冷えるにまかせ、室温で一夜間熟成した。懸濁物は、80℃で400mbarに減圧してロータリーエバポレーターで乾燥した。
12gの清浄な120/140USメッシュ(105〜125μm)、十分にカットされた主に8面体形態の合成ダイヤモンドを空気中500℃で1時間加熱して、酸化した表面を生じた。このダイヤモンドを20mlの脱イオン水を加えた200mlの純エタノール中に懸濁した。懸濁を攪拌することで維持した。
Claims (27)
- 酸化物材料と化学結合を形成するガラス質を好む表面を有し、ダイヤモンド、立方晶窒化ホウ素又はこれらの材料の組み合わせである複数の超硬質研磨粒子を供給する工程、非晶質又はナノ結晶性酸化物、水酸化物又はオキソ水酸化物である酸化物前駆体材料を用いて超硬質研磨粒子を被覆する工程、及び被覆した超硬質研磨粒子を熱処理して被覆を乾燥し精製する工程を含む超硬質研磨粒子の被覆方法。
- 被覆した超硬質研磨粒子を処理して、酸化物前駆体材料を、酸化物前駆体材料の酸化物、窒化物、炭化物、酸窒化物、酸炭化物又は炭窒化物、又は酸化物前駆体材料の元素形態、又はそれらの組み合わせに変換する請求項1に記載の方法。
- 超硬質研磨粒子は、該粒子の表面をガラス質を好むようにするために該粒子を表面処理法で処理されたものである請求項1又は2に記載の方法。
- 変換された酸化物前駆体材料は、該酸化物前駆体材料のミクロン、サブミクロン又はナノ粒子サイズ酸化物、窒化物、炭化物、酸窒化物、酸炭化物及び炭窒化物又は元素形態の該酸化物前駆体材料、又はそれらの組み合わせから選択される請求項2又は3に記載の方法。
- 変換された酸化物前駆体材料は、アルミニウム、チタン、ケイ素、バナジウム、ジルコニウム、ニオブ、ハフニウム、タンタル、クロム、モリブデン及びタングステンの酸化物、窒化物、炭化物、酸窒化物、酸炭化物及び炭窒化物、元素形態のモリブデン及びタングステン、及びこれらの材料の適切な組み合わせから選択される請求項2〜4のいずれかに記載の方法。
- 変換された酸化物前駆体材料は、アルミニウム、チタン、ケイ素、バナジウム、ジルコニウム、ニオブ、ハフニウム、タンタル、クロム、モリブデン及びタングステン及びこれらの材料の適切な組み合わせのナノ粒子サイズの化合物である請求項2〜5のいずれかに記載の方法。
- 変換された酸化物前駆体材料は、ナノ粒子サイズの元素形態のタングステン、モリブデン又はこれらの金属の組み合わせ又は合金である請求項2〜5のいずれかに記載の方法。
- 超硬質研磨粒子を液体媒体に懸濁し、適切な化学試薬を入れて、各粒子表面と結合し粒子上に被覆を構築する酸化物前駆体材料を形成する請求項1〜7のいずれかに記載の方法。
- 適切な化学試薬は、少なくとも一種のアルコキサイド又はアルコキサイドのアルコール溶液である請求項8に記載の方法。
- 液体媒体は、水とアルコールのアリコートである請求項8又は9に記載の方法。
- 適切な化学試薬は、水とアルコールのアリコートである請求項8に記載の方法。
- 液体媒体は、少なくとも一種のアルコキサイド又はアルコキサイドのアルコール溶液である請求項8又は11に記載の方法。
- アルコキサイドは、アルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウムから選択される元素のアルコキサイドである請求項9又は12に記載の方法。
- アルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウム元素のアルコキサイドから選択される、二種又はそれ以上のアルコキサイドを液体媒体に入れる請求項9又は10に記載の方法。
- 液体媒体は、アルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウム元素のアルコキサイドから選択される、二種又はそれ以上のアルコキサイドのアルコール溶液を含んで成る請求項11又は12に記載の方法。
- 適切な化学試薬又は液体媒体は、二種又はそれ以上のアルミニウム、チタン、ケイ素、ジルコニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ハフニウム及びイットリウム元素を組み込む混合アルコキサイド化合物又はコンプレックスの溶液である請求項8〜15のいずれかに記載の方法。
- アルコールは、アルコキサイドと同じアルキル基を有する請求項9〜16のいずれかに記載の方法。
- 酸化物前駆体材料被覆は、細孔性である請求項1〜17のいずれかに記載の方法。
- 被覆した超硬質研磨粒子を、空気、真空又は不活性ガス中で温度制御加熱に付して、表面積が大きな細孔性非晶質被覆に付着した残留揮発性不純物を除去する請求項18に記載の方法。
- 被覆した超硬質研磨粒子を、更に熱処理又は焼成に付して、被覆を結晶化し、微粒子又はナノサイズ粒子酸化物セラミックを形成する請求項19に記載の方法。
- 被覆した超硬質研磨粒子を更に熱処理に付して、被覆をガラス質にしてガラスを形成する請求項19に記載の方法。
- 被覆した超硬質研磨粒子を、反応性ガス中で温度制御反応に付して、該被覆材料を非酸化物セラミック又はガラスに変換する請求項18〜21のいずれかに記載の方法。
- 被覆をアンモニアガスと反応させることで窒化物を形成する請求項22に記載の方法。
- 炭素質ガスと水素の混合物中で被覆を反応させることで、炭化物を形成する請求項22又は23に記載の方法。
- メタン又はエタンと水素との混合物中で被覆を反応させることで、炭化物を形成する請求項24に記載の方法。
- 被覆した超硬質研磨粒子を、反応性ガス中で温度制御反応に付して、被覆材料を酸窒化物又は酸炭化物セラミック又はガラスに変換する請求項18〜21のいずれかに記載の方法。
- 酸化物被覆は水素で還元可能であり、酸化物被覆をマイクロ又はナノ粒子サイズ元素又は金属に変換する請求項20に記載の方法。
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