JP2021513495A - 金属炭化物粒子を含む水性懸濁液 - Google Patents
金属炭化物粒子を含む水性懸濁液 Download PDFInfo
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- JP2021513495A JP2021513495A JP2020542361A JP2020542361A JP2021513495A JP 2021513495 A JP2021513495 A JP 2021513495A JP 2020542361 A JP2020542361 A JP 2020542361A JP 2020542361 A JP2020542361 A JP 2020542361A JP 2021513495 A JP2021513495 A JP 2021513495A
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Abstract
Description
前記少なくとも1つの金属炭化物粒子の割合が、前記懸濁液の全重量に対して、30重量%〜95重量%の範囲内である。
i)基材を提供する工程;
ii)本発明の水性懸濁液を提供する工程;
iii)工程ii)からの懸濁液を、工程i)からの基材の表面に塗布する工程;
iv)塗布された懸濁液を乾燥させ、基材の表面にコーティングを形成する工程。
本発明の文脈における「水性懸濁液」では、水が液相として使用される。前記相中には、最大2重量%、好ましくは最大1重量%の他の溶媒が存在してもよい。ただし、「水性懸濁液」の液相は水のみであることが特に好ましい。
液相としての水に加えて、本発明による水性懸濁液はまた、少なくとも1つの金属炭化物粒子、少なくとも1つの分散剤、及び任意の添加剤を含む。記載された数量は、それぞれの場合、懸濁液の全重量(総重量)に基づいており、存在する成分(component)の全重量は、合計で100重量%になる。
本発明の水性懸濁液は、少なくとも1つの金属炭化物粒子と、少なくとも1つの分散剤とを含み、少なくとも1つの金属炭化物粒子の割合は、懸濁液の全重量に対して、30重量%〜95重量%の範囲内である。金属炭化物粒子の割合は、好ましくは懸濁液から揮発性成分を除去することにより決定され、好ましくは懸濁液を水の蒸発温度より高い温度に加熱することにより行われる。金属炭化物粒子の割合は、秤量した量から決定できる。
基材をコーティングするための本発明の方法は、以下の工程を含む:
i)基材を提供する工程;
ii)本発明の水性懸濁液を提供する工程;
iii)工程ii)からの懸濁液を、工程i)からの基材の表面に塗布する工程;
iv)塗布された懸濁液を乾燥させ、基材の表面にコーティングを形成する工程。
v)工程i)において提供された基材を、工程iii)の前に、好ましくは、表面の機械的粗面化、表面の熱的前処理、表面の化学的処理、及びそれらの混合からなる群から選択される手段によって行われる前処理、ならびに、その後の、特に超音波処理によって行われる、洗浄を伴う前処理をする工程;
vi)工程iv)の後に得られたコーティングを焼結する工程。
(1)140〜160℃で2.5〜3.5時間;その後
(2)180〜220℃で1.5〜2.5時間;その後
(3)(2)の温度で2時間保持し;その後
(4)200〜250℃で1.5〜2.5時間;その後
(5)310〜350℃で4.5〜5.5時間;その後
(6)330〜350℃で1.5〜2.5時間;その後
(7)(6)の温度で2時間保持し;その後
(8)380〜420℃で3.5〜4.5時間;その後
(9)430〜470℃で1.5〜2.5時間。
本発明はさらに、本発明の方法により製造可能な被覆基材に関する。
本発明の被覆基材は、炭化物材料として使用される。
分散撹拌機を用いて、水性タンタル炭化物懸濁液を調製した。これは、タンタル炭化物粉末(70重量%、総不純物含有量:300ppm、H.C.Starck)、ポリアクリル酸(0.5重量%、Mw 5000g/mol、Polyscience Europe GmbH)、焼結助剤(シリコンの0.7重量%、H.C.Starck)、消泡剤(2滴のContraspum,Zschimmer und Schwarz)を、蒸留水(28.8重量%)に一度に一段階ずつ添加することにより行った。各個々の成分の添加の間に、使用した、金属炭化物粉末、分散剤、及び添加剤を懸濁液中に均一に分散することを確実にするために、懸濁液を最大15分間、4000回転/分で、撹拌機ユニットで処理した。懸濁液のpHを水酸化ナトリウム溶液でpH8に調整した。タンタル炭化物の割合は、水性懸濁液の全重量に対して70重量%であった。
分散撹拌機を用いて、水性タンタル炭化物懸濁液を調製した。これは、タンタル炭化物粉末(70重量%、総不純物含有量:300ppm、H.C.Starck)、テトラブチルアンモニウムヒドロキシド(0.5重量%、Sigma Aldrich)、焼結助剤(シリコンの0.7重量%、H.C.Starck)、消泡剤(2滴のContraspum、Zschimmer und Schwarz)を、蒸留水(28.8重量%)に一度に一段階ずつ添加することにより行った。各個々の成分の添加の間に、使用した、金属炭化物粉末、分散剤、及び添加剤を懸濁液中に均一に分散することを確実にするために、懸濁液を最大15分間、4000回転/分で、撹拌機ユニットで処理した。懸濁液のpHは7であった。タンタル炭化物の割合は、水性懸濁液の全重量に対して70重量%であった。
Claims (15)
- 少なくとも1つの金属炭化物粒子と、少なくとも1つの分散剤とを含む水性懸濁液であって、
前記少なくとも1つの金属炭化物粒子の割合は、前記懸濁液の全重量を基準として、30重量%〜95重量%の範囲内である、水性懸濁液。 - 前記少なくとも1つの金属炭化物粒子が、チタン、ジルコニウム、ハフニウム、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、シリコンの炭化物、およびそれらの混合物からなる群から選択され、好ましくはタンタル炭化物であり;ならびに
前記少なくとも1つの金属炭化物粒子が、好ましくは0.05〜25μm、より好ましくは0.5〜5μm、特に好ましくは1〜2μmの範囲内の平均粒径を有し、ならびに/あるいは
前記少なくとも1つの金属炭化物粒子が、好ましくは<300ppm、より好ましくは<10ppm、特に好ましくは<1ppmの個々の元素不純物の含有量を有し;ならびに/あるいは
前記分散剤が、好ましくは3000〜10000g/mol、より好ましくは4000〜6000g/molの範囲内の数平均分子量を有するポリアクリル酸、テトラブチルアンモニウムヒドロキシド、およびそれらの混合物からなる群から選択されることを特徴とする請求項1に記載の水性懸濁液。 - 塩基、特に水酸化ナトリウム溶液、消泡剤、特に脂肪アルコールポリアルキレングリコールエーテル、焼結助剤、特にコバルトまたはシリコン、およびそれらの混合物からなる群から選択される少なくとも1つの添加剤を含むことを特徴とする請求項1または2に記載の水性懸濁液。
- 前記金属炭化物粒子の割合が、前記懸濁液の全重量を基準として、40重量%〜90重量%、好ましくは60重量%〜85重量%の範囲内であり;ならびに/あるいは
前記分散剤の割合が、前記懸濁液の全重量を基準として、0.05重量%〜5重量%、好ましくは0.1重量%〜2重量%の範囲内であり;ならびに/あるいは
少なくとも1つの添加剤の割合が、前記懸濁液の全重量を基準として、0重量%〜10重量%、好ましくは0.5重量%〜5重量%の範囲内であることを特徴とする請求項1〜3のいずれか一項に記載の水性懸濁液。 - 以下の工程を含む、基材のコーティング方法:
i)基材を提供する工程;
ii)請求項1〜4のいずれか一項に記載の水性懸濁液を提供する工程;
iii)工程ii)からの前記懸濁液を、工程i)からの前記基材の表面に塗布する工程;
iv)塗布された懸濁液を乾燥させて、前記基材の表面にコーティングを形成する工程。 - 前記基材が、グラファイト、調整された熱膨張係数を有する材料、好ましくは6.5〜7.5×10−6K−1の範囲内に調整された熱膨張係数を有するグラファイト、およびそれらの混合物からなる群から選択されることを特徴とする請求項5に記載の方法。
- さらに、以下の工程を含むことを特徴とする請求項5または6に記載の方法:
v)工程i)で提供された前記基材を、工程iii)の前に、好ましくは、表面の機械的粗面化、表面の熱的前処理、表面の化学的処理、およびそれらの混合からなる群から選択される手段によって行われる前処理、ならびに、その後の、特に超音波処理によって行われる、洗浄を伴う前処理をする工程;
vi)工程iv)の後に得られたコーティングを焼結する工程。 - 工程iii)における前記懸濁液を、塗装、浸漬または噴霧によって塗布することを特徴とする請求項5〜7のいずれか一項に記載の方法。
- 工程iv)を、100〜600℃、好ましくは120〜550℃、より好ましくは145〜455℃の範囲内の温度で実施し、好ましくは工程iv)を5〜40時間、より好ましくは20〜30時間の期間にわたって実施し、乾燥工程iv)において温度を段階的に上昇させることが特に好ましく、以下の温度範囲および時間間隔が最も好ましい:
(1)140〜160℃で2.5〜3.5時間;その後
(2)180〜220℃で1.5〜2.5時間;その後
(3)(2)の温度で2時間保持し;その後
(4)200〜250℃で1.5〜2.5時間;その後
(5)310〜350℃で4.5〜5.5時間;その後
(6)330〜350℃で1.5〜2.5時間;その後
(7)(6)の温度で2時間保持し;その後
(8)380〜420℃で3.5〜4.5時間;その後
(9)430〜470℃で1.5〜2.5時間;
ならびに/あるいは
工程vi)を、2000〜2600℃、好ましくは2100〜2500℃、より好ましくは2200〜2300℃の範囲内の温度で実施し、好ましくは工程vi)を1〜10時間、より好ましくは3〜5時間の期間にわたって実施し;および/または
工程vi)を、500〜900トル、好ましくは600〜800トル、より好ましくは680〜720トルの範囲内の圧力で実施し;および/または
工程vi)を、不活性ガス、好ましくはヘリウム、アルゴン、窒素、およびそれらの混合物からなる群から選択される不活性ガスの下で実施することを特徴とする請求項5〜8のいずれか一項に記載の方法。 - 工程iv)の後および/または工程vi)の前のコーティングの未焼密度が、少なくとも50%、好ましくは少なくとも60%であり;ならびに/あるいは
工程iv)またはvi)の後のコーティングが、300ppm未満、好ましくは1ppm未満の不純物含有量を有し;ならびに/あるいは
工程iv)またはvi)の後のコーティングが、5%未満、好ましくは1%未満の開放気孔率を有することを特徴とする請求項5〜9のいずれか一項に記載の方法。 - 工程iv)またはvi)の後のコーティングの厚さが、20〜500μm、好ましくは50〜400μm、より好ましくは100〜300μmの範囲内であり;ならびに/あるいは
特に分散剤としてのポリアクリル酸の場合、工程iii)の前の前記水性懸濁液のpHが、5〜10、好ましくは7〜8の範囲内であることを特徴とする請求項5〜10のいずれか一項に記載の方法。 - 請求項5〜11のいずれか一項に記載の方法によって製造可能な被覆基材。
- コーティングの厚さが、20〜500μm、好ましくは50〜400μm、より好ましくは100〜300μmの範囲内であることを特徴とする請求項12に記載の被覆基材。
- 炭化物材料としての請求項12または13に記載の被覆基材の使用。
- 結晶成長のための用途、特に物理気相プロセス、エピタキシープロセスにおける用途、および坩堝のための用途における請求項14に記載の使用。
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PCT/EP2019/052235 WO2019154690A2 (de) | 2018-02-06 | 2019-01-30 | Wässrige suspension enthaltend metallcarbid-partikel |
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FI4129956T3 (fi) * | 2021-08-03 | 2023-11-10 | Fraunhofer Ges Forschung | Menetelmä pinnoitettujen alustojen valmistamiseksi sekä pinnoitettu alusta ja sen käyttö |
ES2976110T3 (es) * | 2021-08-03 | 2024-07-23 | Fraunhofer Ges Zur Foerderungder Angewandten Forschung E V | Procedimiento para la producción de sustratos recubiertos así como sustrato recubierto y su uso |
EP4186881A1 (en) * | 2021-11-24 | 2023-05-31 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Producing tantalum carbide layer on technical ceramics using a spray coating and high-temperature sintering process based on aqueous solutions |
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JP2001206771A (ja) * | 2000-01-21 | 2001-07-31 | Asahi Glass Co Ltd | SiC治具およびその製造法 |
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DE102005040157A1 (de) * | 2005-08-25 | 2007-03-01 | Degussa Ag | Paste aus nanoskaligem Pulver und Dispergiermittel |
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JP2001206771A (ja) * | 2000-01-21 | 2001-07-31 | Asahi Glass Co Ltd | SiC治具およびその製造法 |
JP2008501612A (ja) * | 2004-06-08 | 2008-01-24 | トライアンフ,オペレーティング アズ ア ジョイント ヴェンチャー バイ ザ ガバナーズ オブ ザ ユニバーシティ オブ アルバータ,ザ ユニバーシティ オブ ブリティッシュ コロンビア,カールトン | 複合セラミック対象物の形成方法 |
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US20210032169A1 (en) | 2021-02-04 |
SG11202007211UA (en) | 2020-08-28 |
KR20200118162A (ko) | 2020-10-14 |
JP7512200B2 (ja) | 2024-07-08 |
CN111699164A (zh) | 2020-09-22 |
EP3749625A2 (de) | 2020-12-16 |
CA3093224A1 (en) | 2019-08-15 |
EP3749625B1 (de) | 2022-01-19 |
WO2019154690A2 (de) | 2019-08-15 |
EP3984979A2 (de) | 2022-04-20 |
DE102018201771A1 (de) | 2019-08-08 |
EP3984979A3 (de) | 2022-06-29 |
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