CN103553630A - Preparation method of Ti2AlN/TiN functionally gradient material - Google Patents
Preparation method of Ti2AlN/TiN functionally gradient material Download PDFInfo
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- CN103553630A CN103553630A CN201310498151.XA CN201310498151A CN103553630A CN 103553630 A CN103553630 A CN 103553630A CN 201310498151 A CN201310498151 A CN 201310498151A CN 103553630 A CN103553630 A CN 103553630A
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Abstract
The invention relates to a preparation method of a Ti2AlN/TiN functionally gradient material. The preparation method comprises the following steps: selecting Ti, Al and TiN as raw material, uniformly mixing, pelleting, putting in a vacuum hot-pressing furnace, carrying out hot pressed sintering in a vacuum or argon atmosphere at the reaction temperature of 1300 DEG C at the heating rate of 10 DEG C/minute, keeping the temperature for 3 hours to obtain Ti2AlN, crushing, and carrying out ball milling to obtain the Ti2AlN powder; uniformly mixing the Ti2AlN powder and TiN powder, and carrying out layer-by-layer die-filling, wherein the volume percents of the Ti2AlN powder and TiN powder form a change of gradient in the thickness direction; and putting in the hot-pressing furnace, carrying out hot pressed sintering in a vacuum or inert atmosphere at the reaction temperature of 1200-1400 DEG C at the heating rate of 8-20 DEG C/minute under the pressure of 25-40 MPa, and keeping the temperature for 1-3 hours. By using the powders as the raw materials, the method fully utilizes the advantages of the hot pressed sintering technique to synthesize the Ti2AlN/TiN functionally gradient material which has the advantages of high compactness, small porosity and excellent properties.
Description
Technical field
The present invention relates to a kind of Ti
2the preparation method of AlN/TiN Functionally Graded Materials, belongs to technical field of function materials.
Background technology
In recent years, a class has the double carbide of laminate structure or the extensive attention that nitride ceramics has been subject to Materials science worker.They have metal and ceramic premium properties simultaneously.The same with metal, at normal temperatures, there are good heat conductivility and conductivity, there are lower Vickers hardness and higher Young's modulus and shearing modulus, as metal is the same with graphite, can carry out mechanical workout, and at high temperature there is plasticity; Meanwhile, it has the performance of stupalith, has high yield strength, high-melting-point, high thermal stability and good antioxidant property; More meaningfully they have and are even better than graphite and MoS
2self-lubricating property.These compounds can be with unified molecular formula M
n+1aX
nrepresent, wherein M is transition metal, and A is mainly ⅢHe IV family element, and X is C or N.
Ti
2alN is the found novel lamellar ternary compound of the eighties of last century sixties.It has many good characteristics of metal and pottery concurrently, as excellent conduction, thermal conductivity, and workability, good survivability, high-melting-point, high-modulus, high strength and low density (4.31g/cm
3) etc.This is a kind of novel texture/functional materials that is expected to be widely used in the high-tech sectors such as electronic information, new forms of energy, aerospace.
TiN belongs to gap phase, is face-centred cubic structure, and wherein Ti atom occupies site position, and N atom is arranged in face-centred cubic all octahedral interstices, thereby forms NaCl type crystal structure.TiN has beautiful golden colour lustre, and fusing point is up to 2950 ℃, and Vickers' hardness is 20GPa left and right, and chemical stability is good.TiN also has good heat conduction, conductivity, and this has a wide range of applications it in wear-resisting, corrosion-resistant, high-temperature structural material and electric material.
Ti
2alN has the performance of a lot of excellences, but also there is its weak point, as lower in hardness (3.5GPa), acid-proof alkaline is poor, mechanical property is undesirable etc., limited greatly it as structured material and functional materials use range, and TiN is a kind of high strength that has, high rigidity, high temperature resistant, acid and alkali-resistance, anti abrasive feature, have good conduction and heat conductivility, it has a wide range of applications in high-temperature structural material, wear-resisting, corrosion-resistant and electric material, its thermal expansivity of what is more important and Ti simultaneously
2alN is close, therefore at Ti
2in AlN, introduce appropriate TiN particle as wild phase, will contribute to improve Ti
2the performance of AlN material, obtains the matrix material that has both advantages concurrently.Relevant to Ti at present
2the report of AlN/TiN Functionally Graded Materials almost has no disclosed report.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of Ti
2the preparation method of AlN/TiN Functionally Graded Materials.Ti prepared by the inventive method
2alN/TiN Functionally Graded Materials, has overcome Ti
2the shortcomings such as the hardness of AlN is low, and acid resistance is poor, and mechanical property is undesirable, have greatly widened Ti
2the application of AlN.
The present invention provides with technical scheme for solving the problems of the technologies described above:
According to mole proportioning, be that TiN:Ti:Al=1:1:1.03 carries out weigh batching, mix, compressing tablet is well put in vacuum hotpressing stove afterwards, vacuum or argon gas atmosphere are carried out hot pressed sintering, and temperature of reaction is 1300 ℃, and temperature rise rate is 10 ℃/min, insulation 3h, sintering goes out Ti
2alN, broken, ball milling obtains Ti
2alN powder;
Again by Ti
2alN powder and TiN powder layering dress mould, every layer of Ti
2alN powder and TiN powder mix, and along interlayer Ti
2the volume fraction of AlN powder and TiN powder changes in gradient, then puts in hot pressing furnace, and hot pressed sintering under vacuum or inert atmosphere, temperature of reaction is 1200-1400 ℃, and temperature rise rate is 8-20 ℃/min, and pressure is 25-40MPa, insulation 1-3h.
In such scheme, Ti
2alN powder and TiN powder are by proportioning weighing, and by mixing and ball milling, vacuum-drying, sieves, and successively weigh dress mould.The mixing and ball milling time is 8-24h.Mixing and ball milling medium is dehydrated alcohol.
Described inert atmosphere is argon gas.
Ti
2alN powder and TiN powder can divide four layers of dress mould.
Gradient layer material prepared by the inventive method, through-thickness volume fraction changes in gradient, and the microhardness of its material, intensity, impact resistance etc. all change in gradient, and between each layer, combination is good, there is no sharp interface, the possibility that significantly reduces thermal stresses and occur interlayer faults.
Above-mentioned Ti prepared by the inventive method
2alN/TiN Functionally Graded Materials, is prepared by hot-pressing sintering method.Preparation process is: by proportioning weighing; Mixing and ball milling; Vacuum-drying; Sieve; Successively weigh dress mould; Successively precompressed; Sintering; Again with water coolant naturally cooling.The gradient material density preparing is high, and excellent performance can be applied in different environment.
The present invention compared with prior art, has following major advantage and beneficial effect:
Existing technical study be by Ti mostly
2alN/TiN makes matrix material, has no Ti
2alN/TiN makes gradient material.The present invention proposes with hot pressing and sintering technique, TiN to be introduced wherein first, owing to combining the high strength of TiN phase, high rigidity and Ti
2the toughness of AlN phase, ductility and self-lubricating property, and their thermal expansivity is close, and this is preparation Ti
2alN/TiN thermal stresses mitigation type Functionally Graded Materials provides favourable condition.Ti
2alN/TiN Functionally Graded Materials is considered to have application future in high-strength plate armour and high friction environment.When lower use of complex environment (ultrahigh-temperature, large temperature fall etc.), than the uniform material of performance, there are greater advantages.
The present invention is raw materials used simply, easily purchase.The material density of preparing is high, and without interface pollution, interlayer, in conjunction with good, without obvious interface, has promoted the application of this material greatly.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of embodiment 1 material.
Fig. 2 is embodiment 2 sintering curre figure.
Fig. 3 is volume density and the apparent porosity graphic representation of embodiment 2,3 materials.
Fig. 4 is each gradient layer hardness figure of embodiment 2,3 materials.
Embodiment
Ti
2the synthetic selection mol ratio of AlN powder is that TiN:Ti:Al=1:1:1.03 prepares burden, and mixes, and compressing tablet is well put in vacuum hotpressing stove afterwards and carried out hot pressed sintering, and temperature of reaction is 1300 ℃, and temperature rise rate is 10 ℃/min, insulation 3h, and sintering goes out Ti
2alN, broken, ball milling obtains Ti
2alN powder.The Ti of sintering gained
2the XRD figure spectrum of AlN block materials as shown in Figure 1.
The four layers of graded of take are example, and C1 fills a prescription (by volume carrying out proportioning): (TiN)/(0.7TiN-0.3Ti
2alN)/(0.3TiN-0.7Ti
2alN)/(Ti
2alN).First carry out proportion design, after load weighted powder is prepared burden respectively, be placed in ball grinder, with alcohol medium wet ball-milling 12h, then carry out drying and screening, dried powder is successively packed into after graphite grinding tool, carry out hot pressed sintering under Ar atmosphere, sintering temperature is 1300 ℃; 10 ℃/min of temperature rise rate, pressure is 30MPa, insulation 2h.As shown in Figure 2, the microhardness of the sintered compact that obtains changes from rich Ti sintering curre figure
2alN layer is 5.4-12.9GPa to rich TiN layer direction, and relative density is 95.4%, and apparent porosity is 0.011.
The four layers of graded of take are example, and C2 fills a prescription (by volume carrying out proportioning): (0.9TiN-0.1Ti
2alN)/(0.6TiN-0.4Ti
2alN)/(0.3TiN-0.7Ti
2alN)/(Ti
2alN), first carry out proportion design, after load weighted powder is prepared burden respectively, be placed in ball grinder, with alcohol medium wet ball-milling 16h, then carry out drying and screening, dried powder is successively packed into after graphite grinding tool, under vacuum environment, carry out hot pressed sintering, sintering temperature is 1300 ℃; 10 ℃/min of temperature rise rate, pressure is 35MPa, insulation 2h.The microhardness of the sintered compact that obtains changes from rich Ti
2alN layer is 5.7-15.4GPa to rich TiN layer direction, and relative density is 97.9%, and apparent porosity is 0.003.
Claims (6)
1. a Ti
2the preparation method of AlN/TiN Functionally Graded Materials, is characterized in that:
According to mole proportioning, be that TiN:Ti:Al=1:1:1.03 carries out weigh batching, mix, compressing tablet is well put in vacuum hotpressing stove afterwards, vacuum or argon gas atmosphere are carried out hot pressed sintering, and temperature of reaction is 1300 ℃, and temperature rise rate is 10 ℃/min, insulation 3h, sintering goes out Ti
2alN, broken, ball milling obtains Ti
2alN powder;
Again by Ti
2alN powder and TiN powder layering dress mould, every layer of Ti
2alN powder and TiN powder mix, and along interlayer Ti
2the volume fraction of AlN powder and TiN powder changes in gradient, then puts in hot pressing furnace, and hot pressed sintering under vacuum or inert atmosphere, temperature of reaction is 1200-1400 ℃, and temperature rise rate is 8-20 ℃/min, and pressure is 25-40MPa, insulation 1-3h.
2. preparation method according to claim 1, is characterized in that, Ti
2alN powder and TiN powder are by proportioning weighing, and by mixing and ball milling, vacuum-drying, sieves, and successively weigh dress mould.
3. preparation method according to claim 2, is characterized in that, the mixing and ball milling time is 8-24h.
4. preparation method according to claim 2, is characterized in that, mixing and ball milling medium is dehydrated alcohol.
5. preparation method according to claim 1, is characterized in that, described inert atmosphere is argon gas.
6. preparation method according to claim 1, is characterized in that, Ti
2alN powder and TiN powder divide four layers of dress mould.
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| CN201310498151.XA CN103553630A (en) | 2013-10-22 | 2013-10-22 | Preparation method of Ti2AlN/TiN functionally gradient material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400164A (en) * | 2018-11-06 | 2019-03-01 | 西安交通大学 | A kind of MAX phase/nitride ceramics laminated graded composites and its fast preparation method and application |
| CN114505478A (en) * | 2020-11-16 | 2022-05-17 | 中国科学院上海硅酸盐研究所 | TiN-Ni gradient functional material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919794A (en) * | 2006-09-13 | 2007-02-28 | 武汉理工大学 | High-purity compact aluminium titanium nitride block material and preparation method thereof |
| CN100404465C (en) * | 2006-10-30 | 2008-07-23 | 陕西科技大学 | Method for preparing TiN/Al2O3 composite materials |
-
2013
- 2013-10-22 CN CN201310498151.XA patent/CN103553630A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919794A (en) * | 2006-09-13 | 2007-02-28 | 武汉理工大学 | High-purity compact aluminium titanium nitride block material and preparation method thereof |
| CN100404465C (en) * | 2006-10-30 | 2008-07-23 | 陕西科技大学 | Method for preparing TiN/Al2O3 composite materials |
Non-Patent Citations (2)
| Title |
|---|
| YI LIU ET AL.: "Electric current assisted sintering of continuous functionally graded Ti2AlN/TiN material", 《CERAMICS INTERNATIONAL》 * |
| 鲁云 等: "《先进复合材料》", 31 January 2004, 机械工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400164A (en) * | 2018-11-06 | 2019-03-01 | 西安交通大学 | A kind of MAX phase/nitride ceramics laminated graded composites and its fast preparation method and application |
| CN109400164B (en) * | 2018-11-06 | 2020-08-28 | 西安交通大学 | MAX phase/nitride ceramic layered gradient composite material and rapid preparation method and application thereof |
| CN114505478A (en) * | 2020-11-16 | 2022-05-17 | 中国科学院上海硅酸盐研究所 | TiN-Ni gradient functional material and preparation method and application thereof |
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Application publication date: 20140205 |