CN1008723B - Produce the processing method of titanium nitride powder - Google Patents
Produce the processing method of titanium nitride powderInfo
- Publication number
- CN1008723B CN1008723B CN 86104009 CN86104009A CN1008723B CN 1008723 B CN1008723 B CN 1008723B CN 86104009 CN86104009 CN 86104009 CN 86104009 A CN86104009 A CN 86104009A CN 1008723 B CN1008723 B CN 1008723B
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- powder
- raw material
- nitrogen
- titanium
- nitrogenize
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Abstract
The invention belongs to the improvement of process for preparing titanium nitride powder.It is raw material that the preparation technology of the TiN powder that the present invention proposes adopts titanium sponge, at high temperature directly nitrogenize.Adopt this technology can tube chemical industry preface, shortened process, raising nitrogenize thing, reduce and consume, reduce cost, the TiN powder diameter that makes is even, form evenly, foreign matter content is low, can be used as the raw material of the aspects such as fancy alloy, spray material, powder additive, high technology ceramics, electrical equipment contact of sintering metal, senior color sensation.
Description
The invention belongs to the improvement of process for preparing titanium nitride powder.
Titanium nitride is a kind of golden yellow stupalith with senior color sensation.Have fusing point height (3200 ℃), hardness height (about 2000 kilograms/millimeter of Vickers' hardness
2), advantage such as good conductivity, obtained widely aspect a lot of and used.For making high-quality titanium nitride powder, developed the manufacturing process of multiple titanium nitride powder.
Titanium nitride (TiN) powder can adopt metal titanium, titanium hydride pyroprocessing in nitrogen to obtain; Also can in high temperature nitrogen, the method for reduction with carbon titanium dioxide make; Or be that raw material makes with the nitrogen plasma-arc reaction in hydrogen, ammonia atmosphere with the titanium chloride.
With the metal titanium is raw material, at first needs titanium sponge is made metallic titanium powder through hydrogenation, fragmentation, dehydrogenation operation, and nitrogenize obtains the TiN powder under the high temperature more than 1800 ℃ then.Because sintering or fusion take place down in high temperature easily, are difficult to make fine powder, and will pass through several procedures from titanium sponge to making metallic titanium powder.The TiN powder that the reduction with carbon titanium oxide makes in high temperature, nitrogen is because the content height of oxygen and carbon only is suitable for doing not high briquetting of sintered density and stupalith.With the titanium chloride is raw material, makes not only cost height of TiN powder with the nitrogen plasma-arc reaction in hydrogen, ammonia atmosphere, pollution is arranged, and the impurity of powder (especially oxygen level) is subjected to the purity of hydrogen, ammonia, nitrogen to influence bigger and wayward.
With titanium hydride is raw material, handles to get the TiN powder that homogeneous is formed in 1200～1500 ℃ of nitrogen, but can not obtain the micro mist of homogeneous, is easy to generate sintering and fusion.
Proposing with the titanium hydride among the clear 49-3636 of Japan's special permission communique is raw material, handles in 600～1000 ℃ of following nitrogen and makes the TiN powder.The TiN powder that low temperature generates down is unsettled, places air to gradually change.
The characteristics of the manufacturing process of the TiN powder that the Japan clear 51-11600 of special permission communique proposes are: be raw material with the titanium hydride, in 600～1000 ℃ of following nitrogen, handle generating the TiN powder, under 1000～2400 ℃, in neutral gases such as nitrogen, handle obtaining TiN powder stable in the air then.Adopt this technology must make metal titanium hydrogenation, fragmentation make powder earlier, limit dehydrogenation in nitrogen, limit nitrogenize then.Titanium hydride powder generally all is with titanium sponge elder generation hydrogen treatment, is broken into titanium hydride powder then.And be that the nitridation process of raw material must just can carry out under certain hydrogen pressure with the titanium hydride powders, so nitridation process is quite slow.The TiN powder of Sheng Chenging must just can obtain stable TiN powder through pyroprocessing again at low temperatures, and complexity, consumption are greatly so whole operation is long.The TiN powder hydrogen content height that makes only is adapted at the powder metallurgy aspect and uses, should not be as alloy addition.
The objective of the invention is to propose a kind of processing method of the TiN of producing powder, this processing method flow process is short, nitriding rate is high, consume less, cost is low.
Another object of the present invention be the product cut size that makes with technology of the present invention evenly, form evenly, foreign matter content is low.
The preparation technology of the TiN powder that the present invention proposes is to be the direct nitrogenize of raw material with the titanium sponge.Titanium sponge crushing behind certain size, is at high temperature fed the nitrogen nitrogenize, and the TiN after the nitrogenize is broken into the TiN powder that requires granularity.Nitriding temperature is 1000～1600, and nitrogen pressure is 50～200KPa.
The raw material that uses in the technology of the present invention is the titanium sponge of general purity, cleans oven dry according to a conventional method.For making speed of response unlikely slow excessively, titanium sponge crushing is become fritter (less than 50mm).Feed nitrogen then in high temperature reaction stove, nitrogen pressure should remain between 50～200KPa, keeps the regular hour in 1000～1600 ℃ of temperature ranges.Blowing out cooling then is with the material fragmentation of via nitride, the TiN pulverulent product that ball milling becomes to require granularity.
Nitriding temperature can obtain higher nitriding rate when 1300～1600 ℃ of scopes.Nitrogen pressure is too low, and nitriding velocity is slower; Increase nitrogen pressure and can improve nitriding velocity, but certainly will will increase the carrying capacity of body of heater, serve as better with 90～110KPa.The processing parameter of nitridation time during with nitrogenize is relevant, and temperature height, nitrogen pressure greatly then can obtain the TiN powder of identical nitrogen content in the short period of time.
The preparation technology of the TiN powder that the present invention proposes need not to carry out hydrogen treatment, can simplify working process, and has reduced hydrogen cleaning, the various device of air feed and hydrogenation, instrument.
Preparation technology's nitriding velocity of the TiN powder that the present invention proposes is fast.Compare with the technology that with the titanium hydride is raw material, the time of whole requirements of process shortens 1/3 approximately.Nitridation process is difficult for taking place sintering or melting phenomenon.
Can adopt a step high-temperature ammonolysis to make stable TiN powder with the direct nitrogenize of titanium sponge.This powder does not decompose, does not change chemical ingredients and color under 1800 ℃ in carbon, oxygen atmosphere.The powder nitrogen content reaches as high as 22.3%.The foreign matter content of powder is low, wherein major impurity O
2＜0.4%, C≤0.02%, H
2≤ 0.01%.And form evenly.Can be used as the raw material of the aspect such as fancy alloy, spray material, alloy addition, high technology ceramics, electrical equipment contact of sintering metal, crucible, senior color sensation.The Wimet of manufacturing with TiN powder of the present invention has good mechanical property, compares work-ing life with existing Wimet and wear resistance is obviously improved.The crucible that the TiN powder made from technology of the present invention is made does not split after 1700 ℃ of high temperature Quench, with liquid state or gaseous metal calcium, magnesium, rare earth metal and FeO, CaF
2Slag does not react, and has higher chemical stability.With the sputtering target of TiN powder hot-pressing moulding, can and decorate the gold layer coating and use for wearing layer.
Fig. 1 is a nitrogen pressure when being 100KPa, and nitriding temperature is to the influence curve of nitrogenizing reaction in the direct nitriding process of titanium sponge.Ordinate is nitrogenize percentage ratio (%), and abscissa is a nitriding temperature ℃.
Fig. 2 is when 900 ℃ of nitrogenize, and nitrogen pressure is to the influence curve of nitrogenizing reaction in the technology of the present invention.Ordinate is the gain in weight (milligram) of product, and abscissa is nitrogen pressure (KPa).
Further specify the characteristics of this technology with the following example.
Example one is that 98.62% titanium sponge is cleaned oven dry for 3 kilograms with purity, is broken into the fragment less than 50 millimeters, puts into the reaction crucible and is built in SL-7B type (Shanghai Electric Furnace Factory's manufacturing) high temperature reaction stove, vacuumizes, heats up.When reaching 600 ℃, furnace temperature feeds nitrogen.Continuing to be warmed up to 1300 ℃, nitrogen pressure is that 100KPa, 3 hours postcooling of insulation are come out of the stove.With the material of nitrogenize pack into ball grinder ball milling 5 hours, sieve.
With this explained hereafter TiN powder, direct yield is 93%, nitrogen content is 21%, oxygen level is 0.37%, carbon content 0.02%, hydrogeneous 0.01%.The mean particle size of powder is 3.4 microns, 0.4 meter of specific surface
2/ gram.Powder is a cubic system, perfect crystalline.
Example two by the technical process of example one, generates the TiN powder at 700～1600 ℃ of temperature ranges, 50～200KPa pressure range internal reaction respectively with titanium sponge.Temperature and pressure is seen Fig. 1 to the influence of nitrogenizing reaction, 2.When nitrogen pressure was 100KPa, nitriding temperature was 20.2～22.1% in the nitrogen content of 1300～1600 ℃ of following TiN powder, oxygen level＜0.4%.
Claims (2)
1, a kind of processing method of producing titanium nitride powder, comprise that raw material is handled, the high-temperature ammonolysis operation, it is characterized in that said raw material is the titanium sponge of granularity less than 50mm, said high-temperature ammonolysis is at high temperature directly to feed the nitrogen nitrogenize with titanium sponge, nitriding temperature is 1000-1600 ℃, and nitrogen pressure is 50-200KPa.
2, according to the said processing method of producing titanium nitride powder of claim 1, it is characterized in that said nitriding temperature is 1300-1600 ℃, nitrogen pressure is 90-110KPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86104009 CN1008723B (en) | 1986-06-17 | 1986-06-17 | Produce the processing method of titanium nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86104009 CN1008723B (en) | 1986-06-17 | 1986-06-17 | Produce the processing method of titanium nitride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86104009A CN86104009A (en) | 1987-12-30 |
| CN1008723B true CN1008723B (en) | 1990-07-11 |
Family
ID=4802282
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 86104009 Expired CN1008723B (en) | 1986-06-17 | 1986-06-17 | Produce the processing method of titanium nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1008723B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059639C (en) * | 1996-03-14 | 2000-12-20 | 中国科学技术大学 | Process for preparing nm phosphide and nitride by heat synthesis in organic solvent |
| CN108217612A (en) * | 2018-01-30 | 2018-06-29 | 攀枝花学院 | Prepare the method and apparatus of spherical titanium nitride powder |
| CN109437132B (en) * | 2018-12-14 | 2021-06-11 | 中信锦州金属股份有限公司 | Production method of titanium nitride powder |
| CN112475309A (en) * | 2020-12-15 | 2021-03-12 | 江苏金物新材料有限公司 | Method for preparing spherical titanium nitride powder by reaction atomization method |
-
1986
- 1986-06-17 CN CN 86104009 patent/CN1008723B/en not_active Expired
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| Publication number | Publication date |
|---|---|
| CN86104009A (en) | 1987-12-30 |
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