CN103387216B - With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with starch - Google Patents
With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with starch Download PDFInfo
- Publication number
- CN103387216B CN103387216B CN201310320085.7A CN201310320085A CN103387216B CN 103387216 B CN103387216 B CN 103387216B CN 201310320085 A CN201310320085 A CN 201310320085A CN 103387216 B CN103387216 B CN 103387216B
- Authority
- CN
- China
- Prior art keywords
- purity
- powder
- ticn
- ticn powder
- tioso
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000843 powder Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229920002472 Starch Polymers 0.000 title claims abstract description 10
- 239000008107 starch Substances 0.000 title claims abstract description 10
- 235000019698 starch Nutrition 0.000 title claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 12
- 239000010936 titanium Substances 0.000 title abstract description 12
- 229910052719 titanium Inorganic materials 0.000 title abstract description 12
- 229910052799 carbon Inorganic materials 0.000 title abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000004615 ingredient Substances 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000013064 chemical raw material Substances 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of with TiOSO
4the method that titanium source and carbon source prepare TiCN powder is respectively with starch.By TiOSO
4in mass ratio with starch join in deionized water and mix in 1:4 ~ 10, mixed solution at 100 ~ 150 DEG C dry 24 ~ 48 hours, obtained presoma; Presoma is heated to 1300 ~ 2000 DEG C under nitrogen atmosphere or ammonia dissolving atmosphere protection, is incubated and carries out carbothermic reduction and nitrogenize in 1 ~ 2 hour, i.e. obtained TiCN powder; The purity of described chemical reagent and raw material is analytical pure and above purity; The composition of obtained TiCN powder controls by adding proportioning raw materials, and purity and granularity are determined jointly by order of addition(of ingredients) and preparation technology.The inventive method low cost prepares high-purity, superfine Ti CN, compared with the method preparing TiCN, has that raw material mixes, technique is simple, synthesis temperature is low, generated time is short and the feature such as energy-conserving and environment-protective with tradition.
Description
Technical field
The invention belongs to TiCN Preparation Technique of Powders field, particularly one is with TiOSO
4the method that titanium source and carbon source prepare TiCN powder is respectively with starch.
Background technology
TiCN has high-melting-point, high rigidity, high-wearing feature and the special feature such as functional, not only be widely used in the reinforcement etc. of grinding tool, cutting tool and matrix material, also be used widely as energy and material, and have a wide range of applications in new function material.
Superfine Ti CN powder is badly in need of in modern energy industrial development.Tradition TiO
2synthesize TiCN powder with high temperature reduction after carbon solid phase mixing, with low cost but preparation powder thicker; Current superfine Ti CN powder mainly with pure titanium, titanium organism or gaseous titanium compound for raw material, with the technique such as vapour deposition, plasma heating preparation, raw material and process costs high, make superfine Ti CN powder expensive.Investigation and application low cost prepares superfine Ti CN new technology highly significant.
The TiCN powder of current industrialization scale operation is mostly 2 ~ 5 μm, and along with modernization industrial expansion, the especially development of energy industry, increasing to the demand of ultrafine powder TiCN, superfine Ti CN has higher using value, has a extensive future.But existing market supply superfine Ti CN powder because raw materials cost and preparation technology's cost high and expensive.Therefore carry out the research that low cost prepares ultrafine powder TiCN and there is very large realistic meaning.
The preparation of superfine Ti CN powder is the focus of material supply section scholar research, the existing raw material aspect, aspect of research, also has process aspect.But diverse ways has its relative merits for suitability for industrialized production.
Direct carborization is with simple substance carbon, metallic titanium powder (or TiH
2) be raw material, at high temperature, in nitrogen-based atmosphere, the direct contact reacts of reactant generates TiCN, product purity is high, carbon metering than large, technological process is simple.But titanium valve is expensive, the preparation of purification ultrafine titanium powder is more difficult; Reaction process difficulty controls, and the TiCN synthesized needs further grinding broken, causes the purity drop of product, also will purify further, make this legal system obtain large-scale promotion for superfine Ti CN powder.
Carbothermic method is the traditional method of TiCN powder suitability for industrialized production.This technique is with TiO
2for titanium source, be C source with graphite, carbon black, activated carbon etc., under high temperature, nitrogen group protecting atmosphere, TiO
2tiCN powder is generated by C reduction.Advantage is: raw materials cost is low; Technique is simple, and production efficiency is higher; The granularity of TiCN is micron order.But raw material is poor by mechanically mixing homogeneity; TiCN is also easily oxidized.With regard to current production technology, the powder synthesized can not meet the requirement of fine ceramics completely in granularity and purity.
Also have some other method to prepare superfine Ti CN, but generally there is the high organic compound etc. as high pure metal titanium valve, titanium of ingredient requirement; Synthesis technique is complicated, and as needed heating plasma, microwave heating, vapour deposition etc., appointed condition requires the problems such as high, preparation method or complex process or output limited, cause cost high.The TiCN ultrafine powder technology of exploitation high-level efficiency, low cost, remains the emphasis of countries nowadays scientist and business circles research.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of with TiOSO
4the method that titanium source and carbon source prepare TiCN powder is respectively with starch.
Concrete steps are:
(1) by TiOSO
4in mass ratio with starch join in deionized water and mix in 1:4 ~ 10, gained mixed solution at 100 ~ 150 DEG C dry 24 ~ 48 hours, obtained presoma.
(2) presoma obtained for step (1) is heated to 1300 ~ 2000 DEG C under nitrogen atmosphere or ammonia dissolving atmosphere protection, is incubated and carries out carbothermic reduction and nitrogenize in 1 ~ 2 hour, be i.e. obtained TiCN powder.
The purity of described chemical reagent and raw material is analytical pure and above purity.
The composition of the TiCN powder obtained by the present invention controls by adding proportioning raw materials, and the purity of powder and granularity are determined jointly by order of addition(of ingredients) and preparation technology.
The advantage of the inventive method:
(1) be carbon source with starch, with TiOSO
4for titanium source, through carbothermic reduction, low cost prepares high-purity, superfine Ti CN.
(2), compared with the method preparing TiCN with tradition, have that raw material mixes, technique is simple, synthesis temperature is low, generated time is short and the feature such as energy-conserving and environment-protective.
Embodiment
embodiment:
(1) by 1 gram of TiOSO
4join in deionized water with 8 grams of starch and mix, gained mixed solution at 130 DEG C dry 36 hours, obtained presoma.
(2) presoma that step (1) is obtained is heated to 1650 DEG C under nitrogen atmosphere protection; be incubated and carry out carbothermic reduction and nitrogenize in 1.5 hours; i.e. obtained TiCN powder, gained TiCN powder is through the superfine Ti CN powder of testing graininess analysis to be particle diameter be 150 ~ 300 nanometers.
The purity of described chemical reagent and raw material is analytical pure.
Claims (2)
1. prepare a method for TiCN powder, it is characterized in that concrete steps are:
(1) by TiOSO
4in mass ratio with starch join in deionized water and mix in 1:4 ~ 10, gained mixed solution at 100 ~ 150 DEG C dry 24 ~ 48 hours, obtained presoma;
(2) presoma obtained for step (1) is heated to 1300 ~ 2000 DEG C under nitrogen atmosphere or ammonia dissolving atmosphere protection, is incubated and carries out carbothermic reduction and nitrogenize in 1 ~ 2 hour, be i.e. obtained TiCN powder;
Use the purity of raw material to be analytical pure and above purity.
2. the method preparing TiCN powder according to claim 1, is characterized in that: the composition of obtained TiCN powder controls by adding proportioning raw materials, and the purity of powder and granularity are determined jointly by order of addition(of ingredients) and preparation technology.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310320085.7A CN103387216B (en) | 2013-07-28 | 2013-07-28 | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with starch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310320085.7A CN103387216B (en) | 2013-07-28 | 2013-07-28 | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with starch |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103387216A CN103387216A (en) | 2013-11-13 |
| CN103387216B true CN103387216B (en) | 2016-03-02 |
Family
ID=49531653
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310320085.7A Active CN103387216B (en) | 2013-07-28 | 2013-07-28 | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with starch |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103387216B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115872443A (en) * | 2021-09-29 | 2023-03-31 | 溧阳天目先导电池材料科技有限公司 | Preparation method of nano titanium oxide and nano titanium oxide prepared by same |
| CN115872369A (en) * | 2021-09-29 | 2023-03-31 | 溧阳天目先导电池材料科技有限公司 | Preparation method of nano titanium nitride and prepared nano titanium nitride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462722A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium carbide ceramic powder |
| CN101863663A (en) * | 2010-07-15 | 2010-10-20 | 武汉工程大学 | Combustion method for preparing submicron grade titanium carbide polycrystal powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130506B (en) * | 2013-03-15 | 2014-07-09 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing superfine titanium carbonitride |
-
2013
- 2013-07-28 CN CN201310320085.7A patent/CN103387216B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462722A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium carbide ceramic powder |
| CN101863663A (en) * | 2010-07-15 | 2010-10-20 | 武汉工程大学 | Combustion method for preparing submicron grade titanium carbide polycrystal powder |
Non-Patent Citations (4)
| Title |
|---|
| Carbothermal Reduction Synthesis of Superfined TiC Powders From TiOSO4;Jie Li;《Advanced Materials Research》;20111218;第415-417卷;510-513 * |
| NaBr-KCl和不同炭源对合成Ti(C,N)粉末的影响;陈希来等;《耐火材料》;20070630;第41卷(第6期);413-416 * |
| 以酚醛树脂为碳源碳热还原制备TiC的研究;李鹏飞等;《硅酸盐通报》;20121031;第31卷(第5期);1312-1316 * |
| 高钛渣提取碳氮化钛的研究;李慈颖等;《钢铁钒钛》;20060930;第7页右栏第2段以及第2.2节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103387216A (en) | 2013-11-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104261360B (en) | A kind of beta-silicon nitride powder based on catalysis nitridation and preparation method thereof | |
| CN101125653B (en) | Method for synthesizing homogeneous nano silicon carbide powder by combustion | |
| Zhang et al. | Microwave-aided synthesis of BiOI/g-C3N4 composites and their enhanced catalytic activities for Cr (VI) removal | |
| CN110227826A (en) | A method of preparing high-purity nm molybdenum powder | |
| CN103466701A (en) | Method for preparing bismuth trioxide nanowires by using solid-phase chemical reaction | |
| CN103274409A (en) | Method for preparing superfine TiC powder respectively by using TiOSO4 and phenolic resin as titanium source and carbon source | |
| CN102909030B (en) | Ferrous oxide-based ammonia synthesis catalyst | |
| CN103664194A (en) | Method for preparing non-oxide ceramic ultrafine powder based on solvent thermal polymerization reaction | |
| CN109248695A (en) | A kind of Bi base shape fixed nitrogen photochemical catalyst and preparation method thereof that Lacking oxygen mediates | |
| CN103387216B (en) | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with starch | |
| CN103387215B (en) | The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and starch | |
| CN103466584A (en) | Method for preparing silver phosphate nanometer material by solid phase chemical reaction | |
| CN103496679B (en) | A kind of beta-silicon nitride powder and preparation method thereof | |
| CN103395755B (en) | The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and resol | |
| CN107413361B (en) | Method for preparing non-noble metal tungsten carbide photocatalyst by hydrothermal method | |
| CN103387217B (en) | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with tetramethylolmethane | |
| CN103395754B (en) | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with resol | |
| CN103395753B (en) | The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and tetramethylolmethane | |
| CN103601188B (en) | The preparation method of the carbide of high-melting-point conductive hard ceramic material tantalum | |
| CN103420372B (en) | With TiOSO 4the method that titanium source and carbon source prepare superfine TiC powder is respectively with starch | |
| CN103482693B (en) | The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and pitch | |
| CN103482692B (en) | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with pitch | |
| CN103466622B (en) | With TiOSO 4the method that titanium source and carbon source prepare TiC powder is respectively with pitch | |
| CN103253668B (en) | Low-temperature solid-phase synthesis method for titanium carbide ceramic powder | |
| CN103274408A (en) | Method for preparing superfine TiC powder respectively by using tetrabutyl titanate and starch as titanium source and carbon source |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240425 Address after: 541199 Baoshan High end Equipment Intelligent Manufacturing Industrial Park (Phase I), Lingui District, Guilin City, Guangxi Zhuang Autonomous Region Plant 1 and 2 Patentee after: GUILIN GUIYE HEAVY INDUSTRIES CO.,LTD. Country or region after: China Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin Construction Road No. 12 Patentee before: GUILIN University OF TECHNOLOGY Country or region before: China |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240603 Address after: 541199 Baoshan Industrial Park plot in Liangjiang Town, Lingui District, Guilin City, Guangxi Zhuang Autonomous Region (limited to industrial business activities only); 2 Yaohui, No. 2 Xicheng North Road, Lingui Town, Lingui District, No. 01, 4th to 6th floors, Building 2, Beautiful Home Patentee after: Guilin Guiye High Temperature and High Pressure Machinery Co.,Ltd. Country or region after: China Address before: 541199 Baoshan High end Equipment Intelligent Manufacturing Industrial Park (Phase I), Lingui District, Guilin City, Guangxi Zhuang Autonomous Region Plant 1 and 2 Patentee before: GUILIN GUIYE HEAVY INDUSTRIES CO.,LTD. Country or region before: China |