CN110386819A - A kind of B4C-nanoTiB2The preparation method of diphase ceramic material - Google Patents

A kind of B4C-nanoTiB2The preparation method of diphase ceramic material Download PDF

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CN110386819A
CN110386819A CN201910825310.XA CN201910825310A CN110386819A CN 110386819 A CN110386819 A CN 110386819A CN 201910825310 A CN201910825310 A CN 201910825310A CN 110386819 A CN110386819 A CN 110386819A
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powder
ceramic material
nanotib
diphase ceramic
preparation
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朱品文
王晓楠
贾洪声
陶强
李海波
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Jilin University
Jilin Normal University
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Jilin University
Jilin Normal University
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Abstract

A kind of B of the invention4C‑nanoTiB2The preparation method of diphase ceramic material belongs to diphase ceramic material preparation field.Specific steps are as follows: first by B4C powder and nanometer Ti powder carry out mixing；Then 110 DEG C of briquettings after vacuum heat treatment 2 hours assemble, and finally react 10~30 minutes under the conditions of 4.5GPa~5.5GPa pressure, 1400~1600 DEG C of temperature on cubic hinge press, obtain high tenacity, high rigidity B4C‑nanoTiB2Diphase ceramic material.Method of the invention overcomes B4C‑TiB2Diphase ceramic material is provided simultaneously with the problem of high rigidity and high tenacity, and the synthetic sample time is short, and synthesis temperature is low, tests strong operability, reproducible, so that such material is in military industry field, grinding elements, application prospect is more wide in terms of Structural Engineering material.

Description

A kind of B4C-nanoTiB2The preparation method of diphase ceramic material
Technical field
The invention belongs to diphase ceramic material preparation fields, and in particular to a kind of high tenacity, high rigidity B4C-nanoTiB2It is multiple The high temperature and high pressure preparation process of multiphase ceramics material.
Background technique
Break through boron carbide (B4C high tenacity and high rigidity) is always the hot spot of material educational circles research.Although B4C possesses super High hardness (28-43GPa), and it is widely applied to military, industry and numerous areas, still, B4The lower fracture toughness of C and Extremely difficult agglutinating property significantly limits its many application as functional material.So far, drawn by adding metal binding agent Enter Section 2 particle and carrys out toughening B4C is a kind of more effective method.However, the lower mechanical property of metal binding agent can weaken B4The hardness number of C based composites.For example, in TiB2- 20vol%B4In C-1vol%Ni system, fracture toughness from 2.6MPa·m1/2It is increased to 6.4MPam1/2, but hardness number only has 24.7GPa.Therefore, make B4C based composites have simultaneously Standby high rigidity (>=28GPa) and high tenacity (>=7MPam1/2) challenge is still suffered from, metal binding agent is further studied to B4C Activeness and quietness have very great meaning.
In the B containing metal binding agent4In C system, B4The hardness number of C based composites is between B4C and metal binding agent Between hardness number.Therefore, the mechanical property for improving metal binding agent is the key that enhancing composite material integral hardness.According to Hall Page effect, crystal grain refinement can increase grain boundary density, to improve its mechanical property.In addition, the crystallite dimension of bonding agent from Micron is reduced to the toughness that nanoscale also contributes to improving composite material.Therefore, it is helped using nano metal bonding agent as sintering The B for having high hardness high toughness can be made in agent4C based composites.Up to the present, using the B of nanometer bonding agent4C base complex phase The preparation method of ceramic material mainly has pressureless sintering, hot pressed sintering, sol-gal process etc..These method problems faceds are main Be: pressureless sintering and hot-pressing sintering method require temperature excessively high (2000 DEG C or more), and heating duration is no less than a hour and needs It wants argon gas to protect, is unfavorable for industrialized mass production.Although sol-gal process synthesis temperature is not high, technique is relative complex, And the sample of synthesis does not have excellent mechanical performance report.It can be seen that current preparation high tenacity, high rigidity B4C-nanoTiB2Complex phase pottery The technique of ceramic material needs to be further improved.
Summary of the invention
The purpose of the present invention is to provide a kind of strong operabilitys, have high tenacity, high rigidity B4C-nanoTiB2Complex phase pottery The high temperature and high pressure preparation process of ceramic material.
The specific technical solution of the present invention is as follows:
A kind of B4C-nanoTiB2The preparation method of diphase ceramic material, first by basis material B4C powder and sintering aid material Expect that nanometer Ti powder carries out mixing as sintering original material, wherein B4Molar ratio shared by C powder is shared by 90%~95%, Ti powder Molar ratio is 5%~10%；Then 110 DEG C of briquettings after vacuum heat treatment 2 hours assemble, finally the 4.5GPa on cubic hinge press It is reacted 10~30 minutes under the conditions of~5.5GPa pressure, 1400~1600 DEG C of temperature, obtains high tenacity, high rigidity B4C- nanoTiB2Diphase ceramic material.
Preferably, the basis material B4Purity >=99.9% of C powder, partial size are 2~3 μm；The sintering helps Agent material nanometer Ti powder purity >=99.9%, partial size 60nm.
Preferably, in original material mixed-powder, B4Molar ratio shared by C powder is shared by 95%, Ti powder moles Than being 5%.
Preferably, reaction pressure is 5GPa on cubic hinge press, reaction temperature is 1600 DEG C, and the reaction time is 10 points Clock.
The B of method preparation of the invention4C-nanoTiB2Diphase ceramic material, hardness are higher than 28GPa, and fracture wilfulness is higher than 7MPa·m1/2。
The utility model has the advantages that
1, present invention employs the high temperature and pressure sintering process being produced on a large scale, and under the action of high pressure, connect in particle Driving force is produced between contact, keeps composite material finer and close, while in B4Interface between C crystal grain is generated in-situ to be received Rice TiB2, more uniform is distributed in B4In the matrix of C, the intensity and toughness of composite material are effectively increased.
2, preparation method of the invention does not need protective gas environment, and synthesis temperature is low, tests strong operability, repeats Property it is good, it is primary to complete sintering, the nanometer TiB that reaction in-situ generates2Proportion is smaller in the composite, protects composite material Toughness is significantly improved again while holding high rigidity.This method uses domestic cubic hydraulic press sintetics, process letter List and equipment industrializes extensively, Technical comparing is mature, while greatly shortening generated time, can be realized within 10~30 minutes Densified sintering product, it is easy to accomplish industrialized production.
3, method of the invention overcomes B4C-TiB2Diphase ceramic material is provided simultaneously with the problem of high rigidity and high tenacity, Provide a kind of high tenacity, high rigidity B4C-nanoTiB2The high temperature and high pressure preparation process of diphase ceramic material, the B prepared4C- nanoTiB2Diphase ceramic material compactness is good, and relative density has obtained higher hardness and fracture toughness up to 98% or more Value is respectively 30.9GPa and 7.87MPam1/2.It is wilful much higher than the hardness 24.7GPa of conventional micron grade adhesive and fracture 6.4MPa·m1/2。
Detailed description of the invention
Fig. 1 is the pyrophillite Synthetic block sectional view in Examples 1 to 7.
Fig. 2 is the XRD diagram of sample synthetic sample under the conditions of 5GPa, 10 minutes in embodiment 1,2 and 3.
Fig. 3 is the profile scanning electron microscope of 1 synthetic sample of embodiment.
Fig. 4 is sample hardness test loading force and hardness relation curve in embodiment 1.
Fig. 5 be in embodiment 1,2 and 3 sample hardness and toughness with synthesis temperature change curve.
Fig. 6 be in embodiment 4,5 sample hardness and toughness with synthesis pressure change curve.
Fig. 7 be in embodiment 6,7 sample hardness and toughness with Ti adding proportion change curve.
Specific embodiment
Embodiment 1
Choose the B that partial size is 2~3 μm4For C powder as basis material, shared molar percentage is 95%；Choosing partial size is The Ti powder of 60nm is sintering aid, and shared molar percentage is 5%.After weighing according to the ratio, mixed-powder is first in batch mixer With dehydrated alcohol wet mixing 3h to uniform, 110 DEG C of dry 2h in a vacuum drying oven, then by mixed-powder press compound stalk forming And be fitted into sample cavity, finally it is put into pyrophyllite block by Fig. 1 component.Pyrophyllite block is put into domestic cubic apparatus after component Press (CS-IV, 6 × 14000KN) enterprising horizontal high voltage high―temperature nuclei, experiment condition are 5GPa/1600 DEG C/10min.Experiment obtains Sample having a size of Φ 14mm × 4.5mm, the XRD result of sample as shown in Fig. 2, final product mainly by B4C and TiB2Composition, Since content of graphite is few, composite materials property is influenced negligible.It can by the profile scanning electron microscope of Fig. 3 To find out TiB2Size in 132nm, illustrate that final product is B4C-nanoTiB2Diphase ceramic material, relative density reach 98.66%.Fig. 4 shows that the convergency value of hardness is 30.09GPa, while being 7.87MPa according to the Fracture Toughness that impression calculates m1/2.The hardness of this sample is higher than 28GPa, and fracture is wilful to be greater than 7MPam1/2, it is high hardness high toughness composite material, this is this Optimal conditions in invention.
Embodiment 2
In order to compare the influence of condition of different temperatures, this embodiment is the comparative example of embodiment 1, and experimental temperature is reduced to 1400 DEG C, remaining chooses experiment condition similar to Example 1, that is, the B that partial size is 2~3 μm4C powder as basis material, Shared molar percentage is 95%；Choosing the Ti powder that partial size is 60nm is sintering aid, and shared molar percentage is 5%.It presses After proportion weighs, mixed-powder is first with dehydrated alcohol wet mixing 3h to uniform, 110 DEG C of dryings in a vacuum drying oven in batch mixer Then 2h by mixed-powder press compound stalk forming and is fitted into sample cavity, is finally put into pyrophyllite block by Fig. 1 component.Group Pyrophyllite block is put into domestic cubic hinge press (CS-IV, 6 × 14000KN) enterprising horizontal high voltage high―temperature nuclei after part, is tested Condition is 5GPa/1400 DEG C/10min.Obtained sample is tested having a size of Φ 14mm × 4.5mm block B4C-nanoTiB2Complex phase Ceramic material, relative density reach 98.67%, and hardness number is 28.06GPa (Fig. 5), Fracture Toughness 8.42MPam1/2 (Fig. 5).Therefore it reduces temperature and still shows high rigidity, and due to the reduction of temperature, fracture toughness increases.
Embodiment 3
Temperature is further decreased to 1300 DEG C, remaining chooses experiment condition similar to Example 1, i.e., selection partial size is 2 ~3 μm of B4For C powder as basis material, shared molar percentage is 95%；Choosing the Ti powder that partial size is 60nm is that sintering helps Agent, shared molar percentage are 5%.After weighing according to the ratio, mixed-powder first uses dehydrated alcohol wet mixing 3h extremely in batch mixer Uniformly, then 110 DEG C of dry 2h in a vacuum drying oven by mixed-powder press compound stalk forming and are fitted into sample cavity, most It is put into pyrophyllite block by Fig. 1 component afterwards.After component by pyrophyllite block be put into domestic cubic hinge press (CS-IV, 6 × 14000KN) enterprising horizontal high voltage high―temperature nuclei, experiment condition are 5GPa/1300 DEG C/10min.Obtained sample is tested having a size of Φ 14mm × 4.5mm block B4C-nanoTiB2Diphase ceramic material, relative density reach 98.07%, hardness number 24.71GPa (Fig. 5), Fracture Toughness 9.02MPam1/2(Fig. 5).It can be found that temperature is reduced to 1300 DEG C, although toughness is improved, But hardness number is far below the high rigidity standard of 28GPa, then sample does not have high rigidity under this condition, therefore, keeps high rigidity The reaction temperature lower limit of high tenacity is 1400 DEG C.
Embodiment 4
This embodiment is to compare the influence of pressure, reduction pressure to 4.5GPa, remaining condition same as Example 2, i.e., Choose the B that partial size is 2~3 μm4For C powder as basis material, shared molar percentage is 95%；Choose the Ti that partial size is 60nm Powder is sintering aid, and shared molar percentage is 5%.After weighing according to the ratio, mixed-powder is first with anhydrous second in batch mixer Alcohol wet mixing 3h is to uniform, 110 DEG C of dry 2h in a vacuum drying oven, then by mixed-powder press compound stalk forming and is packed into sample In product chamber, finally it is put into pyrophyllite block by Fig. 1 component.Pyrophyllite block is put into domestic cubic hinge press (CS- after component IV, 6 × 14000KN) enterprising horizontal high voltage high―temperature nuclei, experiment condition is 4.5GPa/1400 DEG C/10min.Test obtained sample Having a size of Φ 14mm × 4.5mm block B4C-nanoTiB2Diphase ceramic material, relative density reach 98.32%, and hardness number is 28.85GPa (Fig. 6), Fracture Toughness 8.28MPam1/2(Fig. 6).Sample still keeps high rigidity and high-ductility under this condition Property.
Embodiment 5
Pressure is further decreased to 4GPa, remaining chooses condition same as Example 2, i.e. selection partial size is 2~3 μm B4For C powder as basis material, shared molar percentage is 95%；Choosing the Ti powder that partial size is 60nm is sintering aid, institute Accounting for molar percentage is 5%.After weighing according to the ratio, mixed-powder first uses dehydrated alcohol wet mixing 3h to uniform, In in batch mixer Then 110 DEG C of dry 2h in vacuum oven by mixed-powder press compound stalk forming and are fitted into sample cavity, finally press Fig. 1 Component is put into pyrophyllite block.Pyrophyllite block is put on domestic cubic hinge press (CS-IV, 6 × 14000KN) after component High pressure-temperature synthesis is carried out, experiment condition is 4GPa/1400 DEG C/10min.Test obtained sample having a size of Φ 14mm × 4.5mm block B4C-nanoTiB2Diphase ceramic material, relative density reach 98.41%, and hardness number is 26.83GPa (Fig. 6), is broken Splitting toughness value is 8.76MPam1/2(Fig. 6).The hardness of sample has been less than 28GPa, therefore high hardness high toughness sample under this condition The low pressure limit of product is 4.5GPa.
Embodiment 6
This embodiment probes into Ti and mixes influence of the ratio to sample hardness and toughness.High Ti molar ratio 8% is chosen, remaining choosing Condition same as Example 1 is taken, that is, chooses the B that partial size is 2~3 μm4C powder is as basis material, shared molar percentage It is 92%；Choosing the Ti powder that partial size is 60nm is sintering aid, and shared molar percentage is 8%.After weighing according to the ratio, mixing Powder first in batch mixer with dehydrated alcohol wet mixing 3h to uniform, 110 DEG C of dry 2h in a vacuum drying oven, then by mixed powder End press compound stalk forming is simultaneously fitted into sample cavity, is finally put into pyrophyllite block by Fig. 1 component.By pyrophillite after component Block is put into domestic cubic hinge press (CS-IV, 6 × 14000KN) enterprising horizontal high voltage high―temperature nuclei, experiment condition 5GPa/1600 ℃/10min.Obtained sample is tested having a size of Φ 14mm × 4.5mm block B4C-nanoTiB2Diphase ceramic material, it is relatively close Degree reaches 98.25%, and hardness number is 28.33GPa (Fig. 7), Fracture Toughness 7.75MPam1/2(Fig. 7).In high Ti ratio Under, sample is likewise supplied with high rigidity and high tenacity.
Embodiment 7
This embodiment reduces Ti molar ratio to 2%, remaining condition and embodiment 1 are consistent, i.e., selection partial size is 2~3 μm B4For C powder as basis material, shared molar percentage is 98%；Choosing the Ti powder that partial size is 60nm is sintering aid, Shared molar percentage is 2%.After weighing according to the ratio, mixed-powder first in batch mixer with dehydrated alcohol wet mixing 3h to uniform, Then 110 DEG C of dry 2h in a vacuum drying oven by mixed-powder press compound stalk forming and are fitted into sample cavity, finally by figure 1 component is put into pyrophyllite block.Pyrophyllite block is put into domestic cubic hinge press (CS-IV, 6 × 14000KN) after component Enterprising horizontal high voltage high―temperature nuclei, experiment condition are 5GPa/1600 DEG C/10min.Test obtained sample having a size of Φ 14mm × 4.5mm block B4C-nanoTiB2Diphase ceramic material, relative density reach 99.95%, and hardness number is 30.43GPa (Fig. 7), is broken Splitting toughness value is 5.44MPam1/2(Fig. 7).Although the sample of low Ti ratio has the high rigidity of 30GPa or more, its is tough Property be lower than 7MPam1/2, therefore, the lower limit of Ti doping is molar ratio 5%.

Claims (4)

1. a kind of B4C-nanoTiB2The preparation method of diphase ceramic material, first by basis material B4C powder and sintering aid material Nanometer Ti powder carries out mixing as sintering original material, wherein B4Molar ratio shared by C powder is to rub shared by 90%~95%, Ti powder You are than being 5%~10%；Then 110 DEG C of briquettings after vacuum heat treatment 2 hours assemble, finally on cubic hinge press 4.5GPa~ It is reacted 10~30 minutes under the conditions of 5.5GPa pressure, 1400~1600 DEG C of temperature, obtains high tenacity, high rigidity B4C-nanoTiB2 Diphase ceramic material.
2. a kind of B according to claim 14C-nanoTiB2The preparation method of diphase ceramic material, which is characterized in that institute The basis material B stated4Purity >=99.9% of C powder, partial size are 2~3 μm；The sintering aid material nano Ti powder purity >= 99.9%, partial size 60nm.
3. a kind of B according to claim 14C-nanoTiB2The preparation method of diphase ceramic material, which is characterized in that In In original material mixed-powder, B4Molar ratio shared by C powder is that molar ratio shared by 95%, Ti powder is 5%.
4. any a kind of B according to claim 1~34C-nanoTiB2The preparation method of diphase ceramic material, feature It is, reaction pressure is 5GPa on cubic hinge press, and reaction temperature is 1600 DEG C, and the reaction time is 10 minutes.
CN201910825310.XA 2019-09-02 2019-09-02 A kind of B4C-nanoTiB2The preparation method of diphase ceramic material Pending CN110386819A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
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Application publication date: 20191029