CN101863663B - Combustion method for preparing submicron grade titanium carbide polycrystal powder - Google Patents
Combustion method for preparing submicron grade titanium carbide polycrystal powder Download PDFInfo
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- CN101863663B CN101863663B CN2010102268308A CN201010226830A CN101863663B CN 101863663 B CN101863663 B CN 101863663B CN 2010102268308 A CN2010102268308 A CN 2010102268308A CN 201010226830 A CN201010226830 A CN 201010226830A CN 101863663 B CN101863663 B CN 101863663B
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Abstract
The invention relates to a combustion method for preparing submicron grade titanium carbide polycrystal powder, which comprises the following steps: mixing organic carbon sources only containing carbon, hydrogen and oxygen with titanium dioxide and metal magnesium powder; carrying out combustion reaction on the mixed materials; and then, carrying out acid washing, water washing, separation and drying on the obtained solid products to obtain the submicron grade titanium carbide polycrystal powder. The invention has the advantages that: (1) the heat effect of the whole reaction system can be regulated and controlled, on one hand, the energy can be saved, on the other hand, the temperature of the self-propagating reaction can be controlled, and the grain growth of the TiC products can be inhibited; (2) the TiC crystal grain sintering and structure glomeration can be perfectly inhibited, and in addition, the invention can be used for isolating product grains, is favorable for forming fine and uniform TiC crystal grains, has high yield, little energy consumption and low cost, and is suitable for large-scale industrial production; and (3) the yield of the titanium carbide is higher than 90 percent, the diameter of the titanium carbide polycrystal grains is between 50 and 250 nm, and the average diameter is 150 nm.
Description
Technical field
The present invention relates to field of ceramic material preparation, concrete relate to a kind of combustion method for preparing submicron grade titanium carbide polycrystal powder.
Background technology
Titanium carbide (TiC) belongs to sodium-chlor type isometric system; Its chemistry and physical properties are stable; Have HMP, high firmness, HS, high-wearing feature and characteristics such as erosion resistance, high-heat resistance shock resistant; Also have good electroconductibility, and since TiC have lower reaction free energy of formation, thereby be a kind of very potential be the hard phase [1] of the particles reiforced metal-base composition of target with wear-resistant grinding abrasion.The mill capacity of TiC can compare favourably with man-made diamond; Its high-wearing feature, low wear rate and have higher intermiscibility with other carbide; Make its application in high-abrasive material particularly outstanding, and in each field, be widely used as new high-abrasive material.TiC mainly is used for making sintering metal, refractory alloy and wimet, and the composite diphase material for preparing with it has a wide range of applications in fields such as mechanical workout, metallurgical mineral products, space industry, fusion reactors.
The method for preparing at present the TiC powder mainly contains carbothermic method, self-propagating high-temperature synthesis method, chemical Vapor deposition process, sol-gel method, microwave process for synthesizing or the like.Li Ciying etc. [2] are raw material with titanium slag, carbon black; The batching of certain proportioning is put plumbago crucible in vertical pyrocarbon pipe furnace and good seal; Carry out carbonization test, made the TiC powder, long reaction time; Owing to receive the influence of diffusion gradient to make the synthetic powder usually pure inadequately, contain unreacted charcoal and TiO in the product in the reaction
2Li Maoxiang [3] is a raw material with tetrabutyl titanate and resol, and EGME is a solvent, and glacial acetic acid is a stablizer, under the catalysis of nitric acid, prepares Gel Precursor, again the presoma that makes is obtained TiC through the pyrocarbon thermal reduction in the ar gas environment of circulation.Liu Yang etc. [4] are raw material with nano titanium oxide and carbon black, with microwave heating synthesis of nano TiC powder.R.Koc etc. [5] are with nano-TiO
2Powder is a raw material, through the thermolysis propylene simple substance inorganic carbon is deposited on TiO
2Increase the contact area of reactant on the powder, thereby the carbothermic reduction reaction temperature is reduced to 1300 ℃, synthesized submicron order high-purity Ti C powder.Li Jingfeng etc. [6] utilize the self-propagating high-temperature synthesis method to prepare the TiC powder in metallic titanium powder-Graphite Powder 99 system, and the self-propagating high-temperature speed of reaction is exceedingly fast, remaining Ti and C simple substance among the TiC.Zhu Xinkun etc. [7] adopt ball milled, are that 1: 1 batching is carried out ball milling by Ti powder and carbon dust mol ratio, with purity greater than 99.9% Ar as shielding gas, made nanocrystal TiC, degree of purity of production is not high yet.After Liu Junbo [8] mixed sphere of powder mill, oven dry with titanium valve and sucrose, carbonization in ebullient oil, generation is deoiled, lighted to oven dry from the synthetic TiC of climing combustion reaction etc. again.
Reference
[1]I.N.Mihailescu，M.L.DeGiorge，C.H.Boulmer-Leborgne，S.Udrea.Direct?carbidesynthesis?by?multipulse?exciter?laser?treatment?of?Ti?sample?in?ambient?CH
4?gas?atsuperatmospheric?Pressure[J]J.APPL.Phys，1994，75：5286-5294
[2] Li Ciying, Li Yawei, Gao Yunming, etc. the research [J] that titanium carbonitride is got in the titanium slag proposition. steel vanadium titanium, 2006,27 (3): 5-9.
[3] Li Maoxiang, Su Guojun. so-gel and carbothermic method prepare the research [J] of titanium carbide. inorganic chemicals industry, 2007,39 (7): 36-38.
[4] Liu Yang, Ceng Keling, Hu Xiaoli, etc. the dynamics research [J] of microwave synthetizing nano titanium carbide powder. Chinese pottery industry, 2003,10 (5): 6-8.
[5]R.Koc，Chang?Meng?and?G.A.Swift.Sintering?properties?of?submieron?TiC?powders?fromcarbon?coated?titania?precursor[J].J.Mater.Sci，2000，35(12)：3131-3141.
[6] Li Jingfeng, Zhang Zhao, Zheng Ziqiao, etc. burning synthetic (TiC, W) forming process of C [J]. rare metal and wimet, 2001,147:1-6.
[7] Zhu Xinkun, Cheng Baochang, Zhang Xiuqing, etc. solid state reaction synthesizes TiC [J]. PM technique, 2001,19 (6): 335-338
[8] Liu Junbo. a kind of preparation method of titanium carbide micro powder [P], Chinese invention patent application 200910014446.9, publication number CN101486462. day for announcing 2009.07.22
[9] Xiang Lunqiang. the mensuration of total carbon, uncombined carbon [J] titanium industrial progress in the carbonized titanium powder, 2004,21 (1): 45-47.
Summary of the invention
Problem to be solved by this invention is to propose a kind of combustion method for preparing submicron grade titanium carbide polycrystal powder to above-mentioned prior art, and its preparation technology is simple, energy consumption is low, is applicable to industrial production.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: combustion method for preparing submicron grade titanium carbide polycrystal powder; It is characterized in that organic carbon source, titanium oxide and the metal magnesium powder of a carbon containing hydrogen-oxygen are mixed, organic carbon source, the metal magnesium powder mole proportioning of titanium oxide, a carbon containing hydrogen-oxygen are TiO
2: C: Mg=1: (0.5～6): (0.5～5); Wherein C is corresponding to carbonaceous mole number in the organic carbon source of carbon containing hydrogen-oxygen; Mixture is through combustion reactions, and the gained solid product can obtain submicron grade titanium carbide polycrystal powder again through pickling, washing, separation and drying.
Press such scheme, the organic carbon source of described titanium oxide, a carbon containing hydrogen-oxygen and metal magnesium powder mole proportion optimization scope are TiO
2: C: Mg=1: (1～4): (0.75～3), wherein C is corresponding to carbonaceous mole number in the organic carbon source of carbon containing hydrogen-oxygen.
Press such scheme, the organic carbon source of described carbon containing hydrogen-oxygen is sucrose, glucose, starch or Hydrocerol A.
Press such scheme, organic carbon source the best of described carbon containing hydrogen-oxygen is a sucrose.
Press such scheme, the organic carbon source of described carbon containing hydrogen-oxygen, titanium oxide and metal magnesium powder are 100～300 order pressed powders.
Press such scheme, described combustion reactions is with mixture direct heating to 700～850 ℃ and the combustion reactions that causes.
Press such scheme, described combustion reactions is that mixture is passed through briquetting, and making the gained block reach density is 1.00～1.15g/cm
3, light block and the reaction of the self-propagating combustion that causes with the hot tungsten filament of energising at normal temperatures then.
Press such scheme; Described pickling, washing, separation and dry concrete steps are: with the 100g solid product; 35～38wt% the concentrated hydrochloric acid that adds 450～800ml stirred 12～24 hours down at 50～80 ℃; Suction filtration is washed with distilled water to neutrality then, and filter cake was in 80 ℃ of following vacuum-dryings 12～24 hours.
Press such scheme, described submicron grade titanium carbide polycrystal powder diameter is 50～250nm.
Among the present invention, the organic carbon source of a metal magnesium powder and a carbon containing hydrogen-oxygen is (with sucrose (C
12H
22O
11) be example), TiO
2The reaction process of magnesiothermic reduction reaction synthesizing submicron TiC powder be exothermic process, shown in (1).Organic carbon source raw material and TiO
2The synthetic TiC of carbothermic reduction reaction be endothermic process, shown in (2).The above-mentioned two reactions net reaction comprehensive by generating equivalent TiC is suc as formula shown in (3):
1/12C
12H
22O
11+TiO
2+2Mg＝TiC+2MgO+11/12H
2O↑ (1)
1/6C
12H
22O
11+TiO
2＝TiC+11/6H
2O↑+CO↑ (2)
1/4C
12H
22O
11+2TiO
2+2Mg＝2TiC+2MgO+11/12H
2O↑+CO↑ (3)
To above-mentioned reaction formula (1)～(3) calculate the mark condition under reaction heat be respectively Δ
rH
θ 1=-525.6kJ/mol, Δ
rH
θ 2=291.7kJ/mol, Δ
rH
θ=-116.9kJ/mol. this shows that a large amount of heat is emitted in magnesiothermic reduction reaction (formula (1)), and carbothermic reduction reaction (formula (2)) is thermo-negative reaction, and two reactions then are thermopositive reaction by generating the comprehensive net reaction (formula (3)) of equivalent TiC.
Generating TiC according to reaction is benchmark, supposes that carbothermic reduction thermo-negative reaction percentage is x% in the whole reaction system, and then magnesiothermic reduction thermopositive reaction percentage is (100-x) %, in the whole reaction system heat effect is so:
Δ
rH
θ＝(100-x)％Δ
rH
θ 1+x％Δ
rH
θ 2 (4)
Visible by equation (4), calculate when x=64.31 Δ in theory
rH
θ=0; Promptly under adiabatic condition; Carbothermic reduction thermo-negative reaction mark is 64.31% o'clock, and whole combustion reactions meeting reaches thermal equilibrium, is not promptly having under the external energy condition; The heat that thermopositive reaction (formula (1)) liberated heat and thermo-negative reaction (formula (2)) absorb equates that the exothermic heat of reaction and the heat absorption of above-mentioned pair of reaction system reach balance.
Can regulate the combustion reactions heat effect through control proportioning raw materials example, even to reach energy-conservation, regulate and control temperature of reaction and more to help the TiC grain refining.
Accompanying drawing 1 provides between different thermo-negative reaction percentage and the total reaction system heat effect and concerns.Can be known that by accompanying drawing 1 under adiabatic condition, the thermo-negative reaction percentage was less than 64.31% o'clock, the total reaction system is the heat release system, i.e. Δ H＜0.
Subordinate list 1 is a combustion method synthesizing submicron titanium carbide product characteristic table look-up.Be to be example for the organic carbon source raw material with sucrose.The data such as severe, TiC product purity of thermo-negative reaction percentage and real reaction have been provided.The thermo-negative reaction percentage is the 0%, the 30%th, the result that self-propagating reaction obtains behind the mixing raw material briquetting, and the thermo-negative reaction percentage is a rate the 0%, 10%, 20%, 30%, the 40%th, the result that the raw material powder combustion reactions obtains.
Table 1. combustion method synthesizing submicron titanium carbide product characteristic table look-up
Fig. 2 is the XRD spectra of submicron order TiC powder; Adopt XD-5A type x-ray powder diffraction instrument (30kV; 20mA; Go into=1.5406
), 2 θ are 10-80 ° of scope).The X-ray diffraction peak of product is consistent with TiC standard diffraction card PDF#89-3828.With thermo-negative reaction percentage in scheming is 0%; The XRD figure spectrum that the mixing raw material dust-firing reacts resultant TiC sample the d value be 2.4820,2.1494,1.5222,1.2972,1.2433
located diffraction peak; Correspond respectively to (111), (200), (220), (311), (222) crystal face of cube TiC; By each crystal face d value of XRD; Calculating the product lattice constant is a=0.4304nm; With standard card a=0.4317nm basically identical, show that product is a cube TiC.With mixing raw material powder self-propagating combustion reaction pair ratio; Obvious wideization of TiC diffraction peak that mixing raw material briquetting self-propagating reaction obtains; And in the reaction of mixing raw material powder self-propagating combustion; Increase with the thermo-negative reaction percentage, the phenomenon of obvious wideization also appears in the TiC diffraction peak, and this explanation mixing raw material briquetting self-propagating reaction and the thermo-negative reaction large percentage synthetic TiC of time institute sample particle are littler.
Beneficial effect of the present invention is: (1) adopts magnesiothermic reduction thermopositive reaction and carbothermic reduction thermo-negative reaction to carry out suitable proportioning; Can regulate and control the heat effect of whole reaction system; On the one hand can be energy-conservation, can control the temperature of self-propagating reaction on the other hand, suppress the grain growing of TiC product; (2) can discharge a large amount of water vapour and CO gas in the reaction process, can take away heat, reduce the combustion system temperature; Can suppress well that TiC is grained sintered to reunite with structure, and can be used for the isolating product particle, help forming tiny and uniform TiC crystal grain; Productive rate is high; Power consumption is few, and cost is low, is fit to large-scale industrial production; (3) titanium carbide yield of the present invention contains uncombined carbon less than 2.75wt% greater than 90% in the described titanium carbide, contains Mg, O and is not higher than 0.5wt%, and the titanium carbide polycrystal particle diameter is 50～250nm, on average is about 150nm.
Description of drawings
Fig. 1 concerns between reaction system heat effect and the thermo-negative reaction percentage;
Fig. 2 is the corresponding XRD spectra of all submicron grade titanium carbide powder samples in the table 1;
Fig. 3 is a solid product pictorial diagram behind embodiment 1 and embodiment 2 mixing raw material dust-firings and the briquetting self-propagating reaction; Wherein Fig. 3 (a) is a solid product pictorial diagram behind the embodiment 1 mixing raw material dust-firing; Fig. 3 (b) is a solid product pictorial diagram behind the embodiment 2 mixing raw material powder compact self-propagating reactions;
Fig. 4 is that embodiment 1 thermo-negative reaction percentage is 0% o'clock TiC sample SEM photo and EDS spectrum;
Fig. 5 is that embodiment 2 thermo-negative reaction percentage are 30% o'clock TiC sample SEM photo.
Embodiment
Further introduce the present invention through embodiment below, but embodiment can not be construed as limiting the invention.Each cited in the technical scheme of the present invention raw material can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention; Do not enumerate embodiment one by one at this.Bound value, the interval value of processing parameter of the present invention (like temperature, time and rotating speed etc.) can both be realized the present invention, do not enumerate embodiment one by one at this.
Embodiment 1
By the thermo-negative reaction percentage is 0%, gets 33.35 gram titanium oxide, 11.91 gram sucrose (C
12H
22O
11), 20.30 gram magnesium powder, mol ratio is TiO
2: C: Mg=1: 1: 2, wherein C was a carbonaceous amount in the organic carbon source raw material, and sucrose, titanium oxide and magnesium powder are 100～300 order pressed powders.Mixing and stirring, direct heating to 800 ℃ generation combustion reactions cools to room temperature with the furnace, and the product after the burning is shown in accompanying drawing 3 (a).Solid product after the burning is with excessive 35wt% salt soak (the 100g solid product adds 650ml hydrochloric acid); In 80 ℃ of following heated and stirred 14 hours; Again through suction filtration and repeatedly washing to neutral; Filter cake obtains black TiC powder 22.88 grams in 80 ℃ of vacuum-dryings 12 hours, is that its yield of benchmark calculating is 91.53% with titanium oxide.
Accompanying drawing 4 is electron scanning micrograph (SEM) and corresponding energy spectrum analysis figure (EDS) of resultant TiC sample; Adopt the S-4800 of Hitachi, Ltd type sem observation granule-morphology and yardstick, characterize elementary composition and content with Horiba 250 model energy spectrometer.Scale length is represented 0.5 μ m in the SEM photo.Visible by photo, the TiC particle fine particle that is obtained is less than 250nm, and the particle mean size is about 150nm.But the TiC sample has tangible sintering and agglomeration, and possibly be that temperature of reaction is too high causes, because the thermo-negative reaction rate is 0%.The massfraction that from the EDS spectrogram, can find out product titaniferous, carbon is respectively 78.40%, 21.01%, contains oxygen and is not higher than 0.16%, contains magnesium and is not higher than 0.43%.From scheming to draw atomic ratio C/Ti=1.07, cause with theoretical value very little reasons of error is arranged mainly possibly be to contain small-amount free carbon in the sample.Adopt chemical separation and high frequency-infrared absorption carbon and sulfur analytical instrument to combine and measure the method [9] of the uncombined carbon in the TiC powder, obtain containing in the sample uncombined carbon 1.25%.
Embodiment 2
According to the thermo-negative reaction percentage is 30%, gets 33.35 gram titanium oxide, 19.06 gram sucrose (C
12H
22O
11), 14.21 gram magnesium powder, mol ratio is TiO
2: C: Mg=1: 1.6: 1.4, wherein C was a carbonaceous amount in the organic carbon source raw material, and sucrose, titanium oxide and magnesium powder are 100～300 order pressed powders.Mixing and stirring, then with the mixture briquetting, it is 1.08g/cm that block reaches density
3, light block and the reaction of the self-propagating combustion that causes with the hot tungsten filament of energising at normal temperatures again, the solid product after the burning is shown in accompanying drawing 3 (b).Solid product is with excessive 35wt.% salt soak (the 100g solid product adds 600ml hydrochloric acid); In 60 ℃ of following heated and stirred 20 hours, again through suction filtration with repeatedly washing is to neutral, filter cake was in 80 ℃ of vacuum-dryings 12 hours; Obtain black TiC powder 23.76 grams; With titanium oxide is that its yield of benchmark calculating is that 95.04%. observes pattern with the sem (SEM) of JSM-5510LV model, and accompanying drawing 5 is SEM photos of resultant TiC sample, and scale length is represented 1 μ m in the photo.The TiC uniform crystal particles, particle diameter 20～100nm, average out to 50nm does not have tangible sintering and aggregation phenomenon.EDS analyzes the massfraction that obtains titaniferous, carbon and is respectively 77.50%, 21.91%, contains oxygen 0.23%, contains magnesium 0.36%, and atomic ratio C/Ti=1.12 records uncombined carbon 1.64%.
Embodiment 3
Get 66.85 gram titanium oxide, 35.62 gram starch (C
6H
12O
6), 34.63 gram magnesium powder, its mol ratio is TiO
2: C: Mg=1: 1.5: 1.7, wherein C was a carbonaceous amount in the organic carbon source raw material, and titanium oxide, starch and magnesium powder are 100～300 order pressed powders.Mixing and stirring, direct heating to 800 ℃ generation combustion reactions cools to room temperature with the furnace.Product product after the burning is with excessive 35wt% salt soak (the 100g solid product adds 700ml hydrochloric acid); In 70 ℃ of following heated and stirred 18 hours; Again through suction filtration and repeatedly washing to neutral; Filter cake obtains black titanium carbide powder 45.52 grams in 80 ℃ of vacuum-dryings 12 hours, is that its yield of benchmark calculating is 91.04% with titanium oxide.Product is analyzed through XRD, SEM, EDS, proves that product is the very high submicron grade titanium carbide polycrystal powder of purity, and particle is less than 250nm, and the particle mean size is 150nm, and particle is thin and even.From the data analysis that EDS provides, the massfraction of product titaniferous, carbon is respectively 77.21%, 22.21%, contains oxygen 0.37%, contains magnesium 0.22%, and atomic ratio C/Ti=1.14 records uncombined carbon 1.75%.
Embodiment 4
Get 50.10 gram titanium oxide, 22.08 gram Hydrocerol A (C
6H
8O
7), 42.67 gram magnesium powder, mol ratio is TiO
2: C: Mg=1: 2.2: 2.8, wherein C was a carbonaceous amount in the organic carbon source raw material, and titanium oxide, Hydrocerol A and magnesium powder are 100～300 order pressed powders.Mixing and stirring, then with the mixture briquetting, it is 1.15g/cm that block reaches density
3, light block and the reaction of the self-propagating combustion that causes with the hot tungsten filament of energising at normal temperatures again.Solid product after the burning is with excessive 35wt% salt soak (the 100g solid product adds 800ml hydrochloric acid); In 80 ℃ of following heated and stirred 12 hours; Again through suction filtration and repeatedly washing to neutral; Filter cake obtains black titanium carbide powder 34.26 grams in 80 ℃ of vacuum-dryings 12 hours, is that its yield of benchmark calculating is 91.36% with titanium oxide.Product is analyzed through XRD, SEM, EDS, proves that product is the very high submicron grade titanium carbide polycrystal powder of purity, and particle is less than 250nm, and the particle mean size is 150nm, and particle is thin and even.From the data analysis that EDS provides, the massfraction of product titaniferous, carbon is respectively 77.99%, 21.61%, contains oxygen 0.16%, contains magnesium 0.24%, and atomic ratio C/Ti=1.10 gets uncombined carbon 1.43%.
Claims (9)
1. the method for combustion method for preparing submicron grade titanium carbide polycrystal powder is characterized in that an organic carbon source of carbon containing hydrogen-oxygen, titanium oxide and metal magnesium powder are mixed, and organic carbon source, the metal magnesium powder mole proportioning of titanium oxide, a carbon containing hydrogen-oxygen are TiO
2: C:Mg=1: (0.5 ~ 6): (0.5 ~ 5); Wherein C is corresponding to carbonaceous mole number in the organic carbon source of carbon containing hydrogen-oxygen; Mixture is through combustion reactions, and the gained solid product can obtain submicron grade titanium carbide polycrystal powder again through pickling, washing, separation and drying.
2. by the method for the described combustion method for preparing submicron grade titanium carbide polycrystal powder of claim 1, it is characterized in that the organic carbon source of described titanium oxide, a carbon containing hydrogen-oxygen and metal magnesium powder mole ratio range are TiO
2: C:Mg=1: (1 ~ 4): (0.75 ~ 3), wherein C is corresponding to carbonaceous mole number in the organic carbon source of carbon containing hydrogen-oxygen.
3. by the method for the described combustion method for preparing submicron grade titanium carbide polycrystal powder of claim 1, the organic carbon source that it is characterized in that described carbon containing hydrogen-oxygen is sucrose, glucose, starch or Hydrocerol A.
4. by the method for the described combustion method for preparing submicron grade titanium carbide polycrystal powder of claim 3, the organic carbon source that it is characterized in that described carbon containing hydrogen-oxygen is a sucrose.
5. by the method for claim 1 or 3 described combustion method for preparing submicron grade titanium carbide polycrystal powder, it is characterized in that organic carbon source, titanium oxide and the metal magnesium powder of described carbon containing hydrogen-oxygen is 100～300 order pressed powders.
6. by the method for the described combustion method for preparing submicron grade titanium carbide polycrystal powder of claim 1, it is characterized in that described combustion reactions is the combustion reactions that mixture direct heating to 700～850 ℃ are caused.
7. by the method for the described combustion method for preparing submicron grade titanium carbide polycrystal powder of claim 1, it is characterized in that described combustion reactions is that mixture is passed through briquetting, making the gained block reach density is 1.00～1.15g/cm
3, light block and the reaction of the self-propagating combustion that causes with the hot tungsten filament of energising at normal temperatures then.
8. press the method for the described combustion method for preparing submicron grade titanium carbide polycrystal powder of claim 1; It is characterized in that described pickling, washing, separation and dry concrete steps are: with the 100g solid product; 35～38 wt% concentrated hydrochloric acids that add 450 ~ 800ml stirred 12～24 hours down at 50～80 ℃; Suction filtration is washed with distilled water to neutrality then, and filter cake was in 80 ℃ of following vacuum-dryings 12～24 hours.
9. by the method for the described combustion method for preparing submicron grade titanium carbide polycrystal powder of claim 1, it is characterized in that described submicron grade titanium carbide polycrystal powder diameter is 50～250 nm.
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| CN103420372B (en) * | 2013-06-01 | 2016-03-02 | 桂林理工大学 | With TiOSO 4the method that titanium source and carbon source prepare superfine TiC powder is respectively with starch |
| CN103387216B (en) * | 2013-07-28 | 2016-03-02 | 桂林理工大学 | With TiOSO 4the method that titanium source and carbon source prepare TiCN powder is respectively with starch |
| CN103387215B (en) * | 2013-07-28 | 2016-03-02 | 桂林理工大学 | The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and starch |
| CN103395755B (en) * | 2013-08-04 | 2015-09-23 | 桂林理工大学 | The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and resol |
| CN103936007A (en) * | 2014-05-05 | 2014-07-23 | 湖南大学 | Method for preparing titanium carbide nano-powder material |
| CN107617441B (en) * | 2017-09-12 | 2020-02-14 | 南京大学昆山创新研究院 | TiO2Polycrystalline foamed ceramic catalyst, preparation method thereof and method for catalyzing waste plastic and biodiesel to produce hydrocarbon by using polycrystalline foamed ceramic catalyst |
| CN113200547A (en) * | 2021-05-24 | 2021-08-03 | 兰州理工大学 | Preparation method of nanoscale TiC powder with controllable macro-particle size |
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