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US4603116A Expired / Lapsed US ⏱️ 0.0 years remaining

Silicon nitride based ceramics and method

Assignee: Verizon Laboratories Inc
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Filing: 1985-09-27
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Granted: 1986-07-29
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Expires: 2005-09-27
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Abstract

Abstract A method of preparing fully dense silicon nitride based ceramic articles comprises the steps of blending a metal oxide component and silicon nitride, wherein a portion of the silicon nitride comprises acicular crystals; comminuting the powder mixture to reduce the aspect ratio of the acicular crystals to an average of less than about 3; pressing the comminuted powder to form a compact; and pressureless sintering the compact to a fully dense ceramic body. Powder mixtures and powder compacts for forming fully dense silicon nitride based ceramic bodies are also disclosed.

Inventors

  • 👤 J. Thomas Smith
  • 👤 Carr Lane W. Quackenbush
  • 👤 Anthony P. Moschetti
  • 👤 Helmut Lingertat

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 15:05
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/515; C04B35/58; C04B35/584

Claims Analysis

Total Claims: 6
Claim 1
Independent Claim 229 words
A method of preparing fully dense silicon nitride base ceramic articles comprising the steps of blending form about 1 to about 25 mole percent of a metal oxide selected from the group consisting of magnesium oxide, aluminum oxide, silicon dioxide, yttrium oxide, the lanthanide rare earth oxides, and mixtures thereof with the balance consisting essentially of silicon nitride including acicular crystals of said silicon nitride; said acicular crystals having an average aspect ratio greater than 3; said acicular crystals being present in sufficient quantity to yield a compact having a green density less than 60% of theoretical; comminuting the blend of metal oxide and silicon nitride to form a powder mixture; monitoring said comminuting to determine the degree of acicularity of said acicular crystals of said silicon nitride, said monitoring comprising removing a sample of said powder mixture being comminuted and pressing said sample into a pill, fracturing said pill forming a fractured surface, examining said fractured surface to determine said degree of acicularity of said acicular crystals; controlling said comminuting to obtain an average aspect ratio of said acicular crystals of said silicon nitride equal to or less than about 3; compacting the comminuted powder mixture to form a green compact having a density of at least 60% of theoretical; and pressureless sintering said compact to form an article having a density of at least 98% of theoretical.
Claim 2
Independent Claim 229 words
A method of preparing fully dense silicon nitride base ceramic articles comprising the steps of blending form about 1 to about 25 mole percent of a metal oxide selected from the group consisting of magnesium oxide, aluminum oxide, silicon dioxide, yttrium oxide, the lanthanide rare earth oxides, and mixtures thereof with the balance consisting essentially of silicon nitride including acicular crystals of said silicon nitride; said acicular crystals having an average aspect ratio greater than 3; said acicular crystals being present in sufficient quantity to yield a compact having a green density less than 60% of theoretical; comminuting the blend of metal oxide and silicon nitride to form a powder mixture; monitoring said comminuting to determine the degree of acicularity of said acicular crystals of said silicon nitride, said monitoring comprising removing a sample of said powder mixture being comminuted and pressing said sample into a pill, fracturing said pill forming a fractured surface, examining said fractured surface to determine said degree of acicularity of said acicular crystals; controlling said comminuting to obtain an average aspect ratio of said acicular crystals of said silicon nitride equal to or less than about 3; compacting the comminuted powder mixture to form a green compact having a density of at least 60% of theoretical; and pressureless sintering said compact to form an article having a density of at least 98% of theoretical.
Claim 3
Dependent Claim 25 words
A method in accordance with claim 1 wherein said step of comminuting comprises ball milling with a milling media-to-charge ratio of 15 to about 30.
Claim 4
Independent Claim 212 words
A method of preparing fully dense silicon nitride based ceramic atricles comprising the steps of comminuting silicon nitride, including acicular crystals of said silicon nitride having an average aspect ratio greater than 3 monitoring said comminuting to determine the degree of acicularity of said acicular crystals of said silicon nitride, said monitoring comprising removing a sample of said powder mixture being comminuted and pressing said sample into a pill, fracturing said pill forming a fractured surface, examining said fractured surface to determine said degree of acicularity of said acicular crystals; controlling said comminuting to obtain an average aspect ratio of said acicular crystals of said silicon nitride equal to or less than about 3; blending from about 1 to about 25 mole percent of a metal oxide selected from the group consisting of magnesium oxide, aluminum oxide, silicon dioxide, yttrium oxide, the lanthanide rare earth oxides, and mixtures thereof with the blance consisting of the comminuted silicon nitride wherein the average aspect ratio of said acicular crystals is equal to or less than about 3; compacting the comminuted powder mixture to form a green compact having a density of at least 60% of theoretical; and pressureless sintering said compact to form an article having a density of at least 98% of theoretical.
Claim 5
Independent Claim 212 words
A method of preparing fully dense silicon nitride based ceramic atricles comprising the steps of comminuting silicon nitride, including acicular crystals of said silicon nitride having an average aspect ratio greater than 3 monitoring said comminuting to determine the degree of acicularity of said acicular crystals of said silicon nitride, said monitoring comprising removing a sample of said powder mixture being comminuted and pressing said sample into a pill, fracturing said pill forming a fractured surface, examining said fractured surface to determine said degree of acicularity of said acicular crystals; controlling said comminuting to obtain an average aspect ratio of said acicular crystals of said silicon nitride equal to or less than about 3; blending from about 1 to about 25 mole percent of a metal oxide selected from the group consisting of magnesium oxide, aluminum oxide, silicon dioxide, yttrium oxide, the lanthanide rare earth oxides, and mixtures thereof with the blance consisting of the comminuted silicon nitride wherein the average aspect ratio of said acicular crystals is equal to or less than about 3; compacting the comminuted powder mixture to form a green compact having a density of at least 60% of theoretical; and pressureless sintering said compact to form an article having a density of at least 98% of theoretical.
Claim 6
Dependent Claim 53 words
A method in accordance to claim 1 wherein said pressureless sintering is done in a nitrogen gas atmosphere having a pressure according to the formula P=e.sup.[(-a/T)+b] where P is the pressure in atmospheres, T is the absolute temperature in degrees Kelvin and a is about 2.9×10 4 , and b is about 15.43.

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1989-07-28 1990-01-27 1990-07-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1993-07-28 1994-01-27 1994-07-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1997-07-28 1998-01-27 1998-07-29 $7700.00 Window Closed / Lapsed

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