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Nanocrystalline α-al 2 o 3 and the preparation method of titanium nitride composite material

A composite material, titanium nitride technology, applied in the field of composite materials, can solve the problems of poor thermal shock resistance, affecting the high temperature performance of materials, and thermal shock resistance, etc., to promote sintering diffusion, reduce sintering temperature, and inhibit grain growth. big effect

Active Publication Date: 2020-09-15
HEBEI VOCATIONAL & TECHN COLLEGE OF BUILDING MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Al 2 o 3 There are two major problems as a refractory material: First, due to the A1 2 o 3 The coefficient of thermal expansion is large and the modulus of elasticity is high, with A1 2 o 3 The thermal shock resistance of the product with the main crystal phase is poor, and the microstructure has an important influence on the thermal shock resistance of the material
However, the introduction of magnesium oxide, calcium oxide, and ferrite will inevitably have an adverse effect on the high-temperature performance of the material
Chinese patent (CN105295451A) discloses a kind of kaolin-nanometer Al with good cohesiveness and strength 2 o 3 The preparation method of the composite material, but the addition of sodium dihydrogen phosphate and aluminum phosphate will also affect the high temperature performance of the material
[0006] Literature "α-Al 2 o 3 Low-temperature preparation of nanoparticles and their sintering characteristics" (Master's thesis of Lanzhou University; Guo Ruiyun; 2016.6) α-Al prepared by precipitation method 2 o 3 Nanoparticles (average particle size 9nm, size distribution 2-27nm), dense α-Al 2 o 3 Nanocrystalline ceramics (average grain size is 55nm), but part of the auxiliary phase α-Fe remains 2 o 3 , which will also affect the high temperature performance of the material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] step 1

[0024] Select α-Al with a particle size of about 3 μm 2 o 3 , non-stoichiometric titanium nitride (TiN 0.3 ); among them, α-Al 2 o 3 80% by volume, TiN 0.3 The volume ratio is 20%.

[0025] step 2

[0026] Weigh the two powders according to the ratio in step 1, and put them into a planetary ball mill tank. This operation process should be completed in a glove box filled with argon. Both the ball mill pot and the grinding medium are made of WC; the ball-to-material ratio is 20:1, the mass of the ball is 800g, the ball diameter is 3-9mm, and the ratio of large, medium and small balls is 3:1:1; the speed of the ball mill is 450rpm; The time is 30h, every 2h shut down for 30min to dissipate heat.

[0027] step 3

[0028] The nano-powder (average particle size 25nm) obtained in step 2 is packed into a graphite grinding tool, and simply pre-pressed on a hydraulic press with a pressure of about 2 MPa.

[0029] step 4

[0030]Place the assembled block obtain...

Embodiment 2

[0034] step 1

[0035] Select α-Al with a particle size of about 3 μm 2 o 3 , non-stoichiometric titanium nitride (TiN 0.3 ); among them, α-Al 2 o 3 70% by volume, TiN 0.3 The volume ratio is 30%.

[0036] step 2

[0037] Weigh the two powders according to the ratio in step 1, and put them into a planetary ball mill tank. This operation process should be completed in a glove box filled with argon. Both the ball mill pot and the grinding medium are made of WC; the ball-to-material ratio is 20:1, the mass of the ball is 800g, the ball diameter is 3-9mm, and the ratio of large, medium and small balls is 3:1:1; the speed of the ball mill is 450rpm; The time is 40h, every 2h shut down for 30min to dissipate heat.

[0038] step 3

[0039] The nano-powder (average particle size 19nm) obtained in step 2 is packed into a graphite grinding tool, and simply pre-pressed on a hydraulic press with a pressure of about 2 MPa.

[0040] step 4

[0041] Place the assembled block obtai...

Embodiment 3

[0045] step 1

[0046] Select α-Al with a particle size of about 3 μm 2 o 3 , non-stoichiometric titanium nitride (TiN 0.4 ); among them, α-Al 2 o 3 75% by volume, TiN 0.4 The volume ratio is 25%.

[0047] step 2

[0048] Weigh the two powders according to the ratio in step 1, and put them into a planetary ball mill tank. This operation process should be completed in a glove box filled with argon. Both the ball mill pot and the grinding medium are made of WC; the ball-to-material ratio is 20:1, the mass of the ball is 800g, the ball diameter is 3-9mm, and the ratio of large, medium and small balls is 3:1:1; the speed of the ball mill is 450rpm; The time is 30h, every 2h shut down for 30min to dissipate heat.

[0049] step 3

[0050] The nano-powder (average particle size 23nm) obtained in step 2 is packed into a graphite grinding tool, and is simply pre-pressed on a hydraulic press with a pressure of about 2 MPa.

[0051] step 4

[0052] Place the assembled block ob...

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Abstract

The invention relates to a preparation method of a nanocrystalline alpha-Al2O3 and titanium nitride composite material. The alpha-Al2O3 having the particle size being 1-3 [mu]m accounts for 70-80 vol% in the composite material, the nonstoichiometric titanium nitride (TiNX, X is greater than or equal to 0.3 and less than or equal to 0.6) accounts for 20-30 vol% in the composite material, two raw materials enable high energy ball milling through a planetary bowl mill, the rotating speed is 450 rpm, and the ball milling time is 30-60 h; the mixed powder is subjected to spark plasma sintering, the sintering temperature is 1300-1500 DEG C, and the insulation time is 10-20 min. The powder after high energy ball milling can reach a nano level, and two materials are highly dispersed, the nano TiNx is dispersed and distributed around the nano alpha-Al2O3 particles, during a sintering process, the pinning effect is effective generated, TiNx has N vacancy defect, the alpha-Al2O3 sintering diffusion is promoted, and the sintering temperature is reduced. The thermal shock resistance and the sintering property of the Al2O3 material are obviously improved.

Description

technical field [0001] The invention relates to the field of composite materials, in particular to a nanocrystalline α-Al 2 o 3 And the preparation method of titanium nitride composite material. Background technique [0002] Al 2 o 3 There are two major problems as a refractory material: First, due to the A1 2 o 3 The coefficient of thermal expansion is large and the modulus of elasticity is high, with A1 2 o 3 The thermal shock resistance of the product with the main crystal phase is poor, and the microstructure has an important influence on the thermal shock resistance of the material. The main methods to improve the thermal shock resistance of materials are: (1) thermal expansion mismatch; (2) particle dispersion; (3) zirconia phase transformation toughening; (4) fiber / whisker toughening and strengthening; (5) in-situ Growth self-reinforcement and toughening; (6) nanoparticle toughening and strengthening. Second, A1 2 o 3 The structure of the bond determines th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/117C04B35/645
CPCC04B35/117C04B35/6455C04B2235/3886C04B2235/77C04B2235/781
Inventor 乔丽娜
Owner HEBEI VOCATIONAL & TECHN COLLEGE OF BUILDING MATERIALS
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