CN106083057A - A kind of silicon carbide-matrix multiphase ceramics material and preparation method thereof - Google Patents

A kind of silicon carbide-matrix multiphase ceramics material and preparation method thereof Download PDF

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CN106083057A
CN106083057A CN201610410680.3A CN201610410680A CN106083057A CN 106083057 A CN106083057 A CN 106083057A CN 201610410680 A CN201610410680 A CN 201610410680A CN 106083057 A CN106083057 A CN 106083057A
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silicon carbide
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multiphase ceramics
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陈健
陈军军
黄政仁
陈忠明
刘学建
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Shanghai Institute of Ceramics of CAS
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Abstract

The present invention relates to a kind of silicon carbide-matrix multiphase ceramics material and preparation method thereof, described silicon carbide-matrix multiphase ceramics material includes silicon carbide substrate material and ZrB2Second phase material, described ZrB2The content of the second phase material is >=20wt%, preferably 20～40wt%.SiC base complex phase ceramic prepared by the present invention has linear C-V characteristic, adjustable resistivity, has higher intensity and hardness and relatively low density simultaneously, is expected to obtain important application at aspects such as realizing the structure resistive element with function integration.Therefore SiC/ZrB2Complex phase ceramic is expected to become the electronics industry element of structure and the function integration that can run under the severe rugged environment such as superhigh temperature, strong acid and strong base.The method of the invention is normal pressure-sintered, can prepare the structural ceramics of difformity and size.

Description

A kind of silicon carbide-matrix multiphase ceramics material and preparation method thereof
Technical field
The present invention relates to the preparation method of a kind of carborundum (SiC) base complex phase ceramic material, belong to SiC ceramic field.
Background technology
Carborundum (SiC) pottery has high intensity, high rigidity, high heat conduction, high temperature resistant, corrosion-resistant, wear-resistant, performance is steady Determine, be difficult to the excellent performances such as aging, be widely used in industrial circle, but SiC ceramic is as a kind of semi-conducting material, Its C-V characteristic is nonlinear, only generally is used as voltage-sensitive ceramic in electronic communication field.
Some part requirement of electronics industry can conducting static electricity there is antiwear characteristic, the most often use surface-coated The alumina material of conductive layer, its life-span is shorter, if replacing with the SiC base complex phase ceramic of linear resistance property, in satisfied use On the basis of requirement, also it is greatly improved the life-span of these industrial parts.
Summary of the invention
For the problems referred to above, it is contemplated that combine SiC ceramic and ZrB2The advantage of pottery, and break through tradition SiC ceramic Pressure-sensitive character, prepare and a kind of there is linear resistance property and the controlled SiC/ZrB of resistivity2Complex phase ceramic, to be applied to Microelectronic.
On the one hand, the invention provides silicon carbide-matrix multiphase ceramics material, described silicon carbide-matrix multiphase ceramics material includes Silicon carbide substrate material and ZrB2Second phase material, described ZrB2The content of the second phase material is >=20wt%, preferably 20～ 40wt%.
The present invention is by ZrB2As the second phase added, ZrB2Be a kind of fusing point and hardness the highest, heat conductivity and electric conductivity Can be good, the anticorrosive and material of ablation.Simultaneously because SiC and ZrB2Thermal coefficient of expansion and elastic modelling quantity suitable, so and The complex phase ceramic that SiC is formed just has good Physical Match, and due to SiC and ZrB2There is not chemical reaction, room temperature Under dissolve each other hardly, the composite ceramics therefore obtained can have the two respective advantage concurrently, therefore with the addition of the second phase ZrB2SiC Base complex phase ceramic can have the two respective advantage concurrently, and its physical and chemical performance has high-temperature stability, intensity is high, density is little, resistance to The characteristics such as corrosion.Work as ZrB2When the content of the second phase material is 20～40wt%, carrier need not intercrystalline Xiao of transition SiC Special base potential barrier, it is only necessary to there is the ZrB of metallic character2Inside conduct.
It is preferred that described silicon carbide-matrix multiphase ceramics material has the linear C-V characteristic of ohmage, work as ZrB2Content When 20-40wt% changes, electricalresistivityρ is 100～102In the range of Ω cm controlled.
It is preferred that the density of described silicon carbide-matrix multiphase ceramics material is 3.48～3.65g cm-3, bending strength is 284 ～325MPa.
On the other hand, present invention also offers the preparation method of a kind of silicon carbide-matrix multiphase ceramics material, including:
Configuration raw material powder: include that SiC powder body that mass percent is 60～80wt% and mass percent are 20～40wt% ZrB2Powder body；
Described raw material powder is mixed by ball milling, is made into the slurry that solid content is 40～45wt%；
By gained slurry mist projection granulating, carry out dry-pressing formed and isostatic pressing successively or directly carry out isostatic pressing, it is thus achieved that Base substrate；After gained base substrate vacuum unsticking, sinter 1～2 hour at 1900～2300 DEG C under normal pressure inert atmosphere conditions, Described silicon carbide-matrix multiphase ceramics material.
It is preferred that the particle diameter of described SiC powder body is 0.1～1 μm.
It is preferred that the particle diameter of described ZrB powder body is 1～5 μm.
It is preferred that be additionally added sintering aid in material powder during configuration raw material, described sintering aid is B or B4C.Described The addition quality of sintering aid is SiC powder body and ZrB2Below the 1wt% of powder body gross mass.
It is preferred that be additionally added binding agent in material powder during configuration raw material, described binding agent is phenolic resin, polyethylene At least one in alcohol (PVA), polyvinyl butyral resin (PVB).The addition quality of described binding agent is SiC powder body and ZrB2Powder The 5～10wt% of body gross mass.
It is preferred that described dry-pressing formed pressure is 10～100MPa, the pressure of described isostatic pressed is 150～210MPa.
A kind of method that present invention also offers resistivity regulating silicon carbide-matrix multiphase ceramics material, with B or B4In C At least one is as sintering aid, with phenolic resin or/and PVA and/or PVB prepares carborundum for binding agent without pressing solidly phase sintering Base complex phase ceramic material, by controlling ZrB2The content of the second phase material is to regulate the resistivity of silicon carbide-matrix multiphase ceramics material So that its electricalresistivityρ is 100～102Ω cm is controlled.
To sum up the SiC base complex phase ceramic prepared by the present invention has linear C-V characteristic, adjustable resistivity, has simultaneously There are higher intensity and hardness and relatively low density, are expected at aspects such as realizing the structure resistive element with function integration To important application.Therefore SiC/ZrB2Complex phase ceramic is expected to become and can run under the severe rugged environment such as superhigh temperature, strong acid and strong base Structure and the electronics industry element of function integration.The method of the invention is normal pressure-sintered, can prepare difformity and chi Very little structural ceramics.
Accompanying drawing explanation
Fig. 1 is different ZrB2Content SiC base complex phase ceramic VA characteristic curve；
Fig. 2 is 18wt%ZrB2The VA characteristic curve of the SiC base complex phase ceramic of content.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that following embodiment is merely to illustrate this below by way of following embodiment Invention, and the unrestricted present invention.
The present invention is can tolerate the conductivity ceramics ZrB of superhigh temperature2It is raw material with SiC, it is desirable to provide a kind of silicon carbide-based multiple Multiphase ceramics material, described silicon carbide-matrix multiphase ceramics material includes silicon carbide substrate material and ZrB2Second phase material, described ZrB2 The content of the second phase material is >=20wt%, preferably 20～40wt%.Work as ZrB2When second phase material content is less than 20wt%, The C-V characteristic of silicon carbide-matrix multiphase ceramics material shows the nonlinear characteristic of varistor.Carrier (electronics or hole) At the intercrystalline Schottky barrier of SiC and ZrB2In ohmage, conduction, shows as nonlinear characteristic.When by burning mutually without pressing solidly Knot and control ZrB2The content of the second phase material is to regulate the resistivity of silicon carbide-matrix multiphase ceramics material to make it have Europe The linear C-V characteristic of nurse resistance.SiC is semi-conducting material, has nonlinear resistance property；ZrB2There is metallic character, to SiC ceramic is added ZrB2, when reaching certain content, SiC ceramic will turn on.Add ZrB2Can be by the volt-ampere of SiC ceramic Characteristic is changed to linear by non-linear.ZrB2Content be about 20wt% be switching point, remain non-linear less than 20wt% Resistor ceramic, more than 20wt% becomes linear resistor ceramic.Work as ZrB2Content is when 20-40wt% changes, and electricalresistivityρ is 100 ～102In the range of Ω cm controlled.Along with the second phase material ZrB2Content the most, its resistance will be the least.That is, the present invention can With by regulation ZrB2Content regulate the electrology characteristic of SiC ceramic.
The illustrative fabrication process of the silicon carbide-matrix multiphase ceramics material of the present invention is described below.The present invention with SiC powder body, ZrB2Powder body, sintering aid, binding agent (phenolic resin or/and PVA and/or PVB) are raw material, are made into slurry by ball milling mixing Material.The particle diameter of described SiC powder body can be 0.1～1 μm.The particle diameter of described ZrB powder body can be 1-5 μm.Particle diameter when this scope, powder Body has preferable sintering activity.Wherein, SiC powder body is preferably high-purity alpha-SiC powder body, its oxygen content≤1.8wt%, and Fe content≤ 0.02wt%, in order to avoid the electric property of impact pottery.Count on the basis of the gross weight of solid powder, sintering aid be preferably B and B4At least one in C, weight/mass percentage composition can be 0～1wt%.It is organic that binding agent is chosen as phenolic resin, PVA, PVB etc. Thing, weight/mass percentage composition can be 5～10wt%, it is possible to as required binding agent wiring solution-forming is added when ball milling mixes.At ball Can be selected for SiC ball during mill mixing as mill ball, using ensure in mechanical milling process that mill ball damages material will not be as new impurity raw material Occurring, wherein SiC ball quality and raw material powder mass ratio can be 2:1.Water or other solvents, last shape is added in mechanical milling process Become powder quality than the slurry being 40～45wt%.
Then slurry mist projection granulating is made powder body, then powder body is made base substrate through dry-pressing formed and isostatic pressing. Dry-pressing formed pressure is chosen as 10～100Mpa, carry out pressure when isostatic pressing processes the most under stress and be chosen as 150 ～210MPa, time 2min.Or directly carrying out isostatic pressing, pressure is chosen as 150～210MPa, time 2min.
After vacuum unsticking, base substrate is sintered under normal pressure inert gas conditions, just can obtain described silicon carbide-based complex phase Ceramic material.Sintering atmosphere is chosen as normal pressure argon gas atmosphere, and sintering temperature is 1900～2300 DEG C, and sintering time is 1～2 little Time.
As an example, it is specifically described low pressure SiC voltage-sensitive ceramic preparation process further, includes the following: 1) configuration Raw material powder: described material powder mainly includes SiC powder body and ZrB2Powder body, wherein the addition of SiC powder body be SiC powder body and ZrB2The 60～80wt% of powder body total amount, ZrB2The addition of powder body is SiC powder body and ZrB2The 20～40wt% of powder body total amount. Can also add sintering aid, the addition of sintering aid is SiC powder body and ZrB2Below the 1wt% of powder body gross mass.Simultaneously Can also add appropriate binding agent, the addition of this binding agent is SiC powder body and ZrB2The 5～10wt% of powder body gross mass； 2) described raw material powder is mixed by ball milling, be made into the slurry that solid content is 40～45wt%；3) spraying of gained slurry is made Grain, carries out dry-pressing formed and isostatic pressing successively or directly carries out isostatic pressing, it is thus achieved that base substrate；4) by gained base substrate vacuum After unsticking, sinter 1～2 hour at 1900～2300 DEG C under normal pressure inert atmosphere conditions, obtain described silicon carbide-based complex phase pottery Ceramic material.The particle diameter of described SiC powder body is 0.1～1 μm, and the particle diameter of described ZrB powder body is 1-5 μm.Described sintering aid be B or B4C.Described binding agent is phenolic resin, PVA, PVB etc..Described dry-pressing formed pressure is 10～100MPa, described isostatic pressed Pressure be 150～210MPa.
SiC base complex phase ceramic materials processing by acquisition becomes the disk of Φ 12mm thickness 2mm, and is polished at its two ends, Its two ends are uniformly coated with and are covered with ag paste electrode, then by its 750 DEG C of insulation 10min in Muffle furnace.
By the SiC ceramic disk of acquisition through Keithley (Keithley) 2450 multiple channel test system test, with ZrB2Contain The increase of amount, its electricalresistivityρ is reduced to 1.94 Ω cm from 220.13 Ω cm, as shown in Figure 1.
The density measuring gained silicon carbide-matrix multiphase ceramics material through Archimedes method is 3.48～3.65g cm-3, through three It is 284～325MPa that some bending method measures gained silicon carbide-matrix multiphase ceramics material bending strength.
Different ZrB is obtained through Keithley (Keithley) 2450 multiple channel test system test2Content normal pressure solid-phase sintering The VA characteristic curve of SiC ceramic is as depicted in figs. 1 and 2.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this Invention is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to this Some nonessential improvement and adjustment that bright foregoing is made belong to protection scope of the present invention.Following example is concrete Technological parameters etc. are the most only that an example in OK range, i.e. those skilled in the art can be done properly by explanation herein In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
SiC、ZrB2(20wt%) 100g, sintering aid B are had altogether4C 0.6g, phenolic resin 10g, powder body is made into solid content is The slurry of 45wt%, with SiC ball 200g as ball-milling medium, mixes 24h.Then drying and screening, the powder body obtained is on purl machine 15MPa pressure forming, then isostatic pressed under 200MPa pressure.Sintering under normal pressure Ar atmosphere after unsticking, sintering temperature is 2100 DEG C, temperature retention time 1h, the SiC base complex phase ceramic density obtained is 3.48g cm-3, bending strength 313MPa.By obtain The sequin of Φ 12mm thickness 2mm made by pottery, and two ends coating ag paste electrode, then by its 750 DEG C of insulation in Muffle furnace 10min, it is thus achieved that electronic component through Keithley (Keithley) 2450 multiple channel test system test, its electricalresistivityρ is 220.13Ω·cm。
Embodiment 2
SiC、ZrB2(24wt%) 100g, sintering aid B are had altogether4C 0.6g, adhesive phenolic resin 8g, be made into powder body and admittedly contain Amount is the slurry of 45wt%, with SiC ball 200g as ball-milling medium, mixes 24h.Then drying and screening, the powder body obtained is at flat board 15MPa pressure forming on machine, then isostatic pressed under 200MPa pressure.Sinter under normal pressure Ar atmosphere after unsticking, sintering temperature Being 1900 DEG C, temperature retention time 2h, the SiC base complex phase ceramic density of material obtained is 3.55g cm-3, bending strength is 310MPa. The pottery of acquisition makes the sequin of Φ 12mm thickness 2mm, and two ends coating ag paste electrode, then by it in Muffle furnace 750 DEG C insulation 10min, it is thus achieved that electronic component through Keithley (Keithley) 2450 multiple channel test system test, its electricalresistivityρ It is 15.37 Ω cm.
Embodiment 3
SiC、ZrB2(28wt%) 100g, sintering aid B are had altogether4C 0.6g, adhesive phenolic resin 5g, be made into powder body and admittedly contain Amount is the slurry of 45wt%, with SiC ball 200g as ball-milling medium, mixes 24h.Then drying and screening, the powder body obtained is at flat board 15MPa pressure forming on machine, then isostatic pressed under 200MPa pressure.Sinter under normal pressure Ar atmosphere after unsticking, sintering temperature Being 2200 DEG C, temperature retention time 1h, the SiC base complex phase ceramic density of material obtained is 3.64g cm-3, bending strength is 316MPa. The pottery of acquisition makes the sequin of Φ 12mm thickness 2mm, and two ends coating ag paste electrode, then by it in Muffle furnace 750 DEG C insulation 10min, it is thus achieved that electronic component through Keithley (Keithley) 2450 multiple channel test system test, its electricalresistivityρ It is 6.89 Ω cm.
Embodiment 4
SiC、ZrB2(40wt%) 100g, sintering aid B are had altogether4C 0.6g, PVA 5g, it is 45wt% that powder body is made into solid content Slurry, with SiC ball 200g as ball-milling medium, mix 24h.Then mist projection granulating, the powder body obtained is 10MPa pressure on purl machine Power molding, then isostatic pressed under 200MPa pressure.Sintering under normal pressure Ar atmosphere after unsticking, sintering temperature is 2300 DEG C, protects Temperature time 2h, the SiC base complex phase ceramic density of material obtained is 3.65g cm-3, bending strength 284MPa.The pottery that will obtain Making the sequin of Φ 12mm thickness 2mm, two ends coat ag paste electrode, then by its 750 DEG C of insulation 10min in Muffle furnace, The electronic component obtained is through Keithley (Keithley) 2450 multiple channel test system test, and its electricalresistivityρ is 1.94 Ω cm.
Fig. 2 is 18wt%ZrB2The VA characteristic curve of the SiC base complex phase ceramic of content, as can be seen from Figure 2 its C-V characteristic Show the nonlinear characteristic of varistor, pressure sensitive voltage U1mA(electric current density 1mA cm-2) it is 1.90V mm-1, non-linear Factor alpha=1.66.
Comparative example 1
SiC、ZrB2(18wt%) 100g, sintering aid B are had altogether4C 0.6g, adhesive phenolic resin 10g, be made into solid by powder body Content is the slurry of 45wt%, with SiC ball 200g as ball-milling medium, mixes 24h.Then mist projection granulating, the powder body obtained is flat 20MPa pressure forming on trigger, then isostatic pressed under 200MPa pressure, sinter after unsticking under normal pressure Ar gas atmosphere, sintering Temperature is 1900 DEG C, temperature retention time 1h, and the SiC base complex phase ceramic density of material obtained is 3.44g cm-3, bending strength is 310MPa.The pottery of acquisition is made the sequin of Φ 12mm thickness 2mm, and two ends coating ag paste electrode, then by it in Muffle In stove 750 DEG C insulation 10min, it is thus achieved that electronic component through Keithley (Keithley) 2450 multiple channel test system test, its C-V characteristic shows the nonlinear characteristic of varistor, pressure sensitive voltage U1mA(electric current density 1mA cm-2) it is 1.90V mm-1, nonlinear factor α=1.66.

Claims (10)

1. a silicon carbide-matrix multiphase ceramics material, it is characterised in that described silicon carbide-matrix multiphase ceramics material includes carborundum Matrix material and ZrB2Second phase material, described ZrB2The content of the second phase material is >=20wt%, preferably 20～40wt%.
Silicon carbide-matrix multiphase ceramics material the most according to claim 1, it is characterised in that described silicon carbide-matrix multiphase ceramics Material has the linear C-V characteristic of ohmage, works as ZrB2Content is when 20wt%-40wt% changes, and electricalresistivityρ is 100～102 In the range of Ω cm controlled.
Silicon carbide-matrix multiphase ceramics material the most according to claim 1 and 2, it is characterised in that described silicon carbide-based complex phase The density of ceramic material is 3.48～3.65g cm-3, bending strength is 284～325MPa.
4. the preparation method of silicon carbide-matrix multiphase ceramics material as according to any one of claim 1-3, it is characterised in that Including:
Configuration raw material powder: include that SiC powder body that mass percent is 60～80wt% and mass percent are 20～40wt% ZrB2Powder body；
Described raw material powder is mixed by ball milling, is made into the slurry that solid content is 40～45wt%；
By gained slurry mist projection granulating, carry out dry-pressing formed and isostatic pressing successively or directly carry out isostatic pressing, it is thus achieved that Base substrate；
After gained base substrate vacuum unsticking, sinter 1～2 hour at 1900～2300 DEG C under normal pressure inert atmosphere conditions, Described silicon carbide-matrix multiphase ceramics material.
Preparation method the most according to claim 4, it is characterised in that the particle diameter of described SiC powder body is 0.1～1 μm.
6. according to the preparation method described in claim 4 or 5, it is characterised in that the particle diameter of described ZrB powder body is 1～5 μm.
7. according to the preparation method according to any one of claim 4 to 6, it is characterised in that at material powder during configuration raw material In be additionally added sintering aid, described sintering aid is B or B4C。
8. according to the preparation method according to any one of claim 4 to 7, it is characterised in that at material powder during configuration raw material In be additionally added binding agent, described binding agent be in phenolic resin, polyvinyl alcohol (PVA), polyvinyl butyral resin (PVB) at least A kind of.
9. according to the preparation method according to any one of claim 4 to 8, it is characterised in that described dry-pressing formed pressure is 15～100MPa, the pressure of described isostatic pressed is 150～210MPa.
10. the method for the resistivity regulating silicon carbide-matrix multiphase ceramics material, it is characterised in that with B or B4In C at least A kind of as sintering aid, with phenolic resin or/and PVA and/or PVB prepares silicon carbide-based multiple for binding agent without pressing solidly phase sintering Multiphase ceramics material, by controlling ZrB2The content of the second phase material with regulation silicon carbide-matrix multiphase ceramics material resistivity so that Its electricalresistivityρ is 100～102Ω cm is controlled.
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