CN105369198A - Chromium-nitride-stabilized zirconium oxide vacuum coating material and manufacturing method thereof - Google Patents
Chromium-nitride-stabilized zirconium oxide vacuum coating material and manufacturing method thereof Download PDFInfo
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- CN105369198A CN105369198A CN201410436747.1A CN201410436747A CN105369198A CN 105369198 A CN105369198 A CN 105369198A CN 201410436747 A CN201410436747 A CN 201410436747A CN 105369198 A CN105369198 A CN 105369198A
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- zirconium oxide
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Abstract
The invention provides a chromium-nitride-stabilized zirconium oxide vacuum coating material and a manufacturing method thereof. Raw materials of the chromium-nitride-stabilized zirconium oxide vacuum coating material comprise, by mole, 75% to 98% of zirconium oxide and 2% to 25% of chromium nitride, and a proper amount of a polyvinyl alcohol bonding agent is added. The manufacturing method of the chromium-nitride-stabilized zirconium oxide vacuum coating material includes the following steps that firstly, zirconium oxide powder and chromium nitride powder serve as the raw materials, the raw materials are weighed according to the selected mole percents and evenly mixed, the polyvinyl alcohol bonding agent is then added, and the powder is agglomerated, pelletized and formed; secondly, the particle materials are pre-sintered, wherein the pre-sintering temperature is 1200 DEG C; and thirdly, the materials are sintered in a vacuum sintering furnace and then naturally cooled to the indoor temperature. By the adoption of the chromium-nitride-stabilized zirconium oxide vacuum coating material, the problems that a traditional zirconium oxide coating material is unstable and the refraction rate of the traditional zirconium oxide coating material is uneven in the coating process are solved, and the damage threshold value of a zirconium oxide film is increased.
Description
Technical field
The present invention relates to a kind of chromium nitride vacuum coating material of stable zirconia and preparation method thereof.
Background technology
Zirconium dioxide membrane has good thermostability, chemical stability and mechanical characteristics.But zirconium dioxide exists polymorphic transition change, the performance of film is had a significant impact.ZrO
2there are three kinds of main crystal formations, i.e. monocline, four directions and cubic.Monoclinic phase is stable existence at room temperature, is heated to 1170 DEG C and changes Tetragonal into, is Emission in Cubic at 2370 DEG C of tetragonal phase convertings, and Emission in Cubic is stabilized to zirconium white fusing point 2680 DEG C always, when cooling, reversible transformation occurs.Because along with 3%-5% volume change between monocline and tetragonal structure change, this can make zirconia material destroy, so ZrO
2film undergoes phase transition generation splash in coating process, makes evaporation line be not easy to control, is difficult to the stability ensureing coating process.Produce a large amount of defect in the film, under the good fortune of laser is shone, this defect becomes absorbent core, and produce heat accumulation, temperature raises rapidly and film is damaged at short notice simultaneously.The specific refractory power of zirconia film has obvious ununiformity in addition, and along with thickness increases, specific refractory power reduces, and due to zirconic above shortcoming, causes the film prepared often cannot reach optical property and the resisting laser damage performance of expection.
At ZrO
2add Y
2o
3as stablizer, due to ZrO
2middle Zr
4+ionic radius and Y
2o
3middle Y
3+ionic radius closely.Y
3+zr in displacement Zr dot matrix
4+and form binary solid solution, be filled with lattice imperfection, inhibit structure distortion, inhibit ZrO
2phase transformation, makes ZrO
2high-temperature-phase (Tetragonal or Emission in Cubic) directly remains into room temperature, eliminates ZrO
2volume effect, to avoid in coating process phase transformation and occur and threshold value is improved.Y
2o
3add the heterogeneity can also eliminating film, specific refractory power is born and is varied down to the degree being enough to ignore, thus the rete of stable refractive index can be obtained.ZrO
2and Y
2o
3all belong to high refractive index Coating Materials, at ZrO
2a small amount of Y is added in coating materials
2o
3, the rete prepared with this compound coating materials and ZrO
2compare, specific refractory power is without obvious decline, and this can not have an impact to the optical property of film.
Summary of the invention
The object of this invention is to provide vacuum coating material of a kind of chromium nitride stabilizing zirconia and preparation method thereof, to solve instability in conventional oxidation zirconium Coating Materials coating process and refractive index inhomogeneity problem, improve the damage threshold of zirconia film.
Object of the present invention is realized by following technical solution:
A vacuum coating material for chromium nitride stabilizing zirconia, it is characterized in that the composition of this material is: raw material mol%, zirconium white 75 ~ 98, chromium nitride 2 ~ 25, polyvinyl alcohol bonding agent is appropriate.
The preparation method of the vacuum coating material of described chromium nitride stabilizing zirconia comprises the following steps:
1. with zirconium white and chromium nitride powder for raw material, by selected molar percentage raw materials weighing, mix rear interpolation polyvinyl alcohol bonding agent and powder reunited, granulating and forming;
2. carry out pre-burning to particulate material, calcined temperature is 1200 DEG C;
3. then sinter in vacuum sintering furnace, vacuum tightness is 1 × 10
-2~ 1 × 10
-4handkerchief, temperature rise rate is 5 ~ 10 DEG C/min, and when sintering temperature is 1700 ~ 2200 DEG C, soaking time is more than 120 minutes, and then naturally cooling is cooled to room temperature.
Described granulating and forming, its granular size is generally 1mm, uses to be suitable for plated film.The invention has the advantages that:
The zirconium white vacuum coating material that chromium nitride of the present invention is stable, due to adding of chromium nitride, Y
3+displacement Zr
4+, both generate sosoloid, make ZrO
2high-temperature-phase can be stabilized to room temperature, make zirconium white volume change not occur, thus do not undergo phase transition in coating process, add the stability of coating process, this just decreases the probability that defect produces to a great extent, improves the threshold for resisting laser damage of material.Add chromium nitride simultaneously and can also eliminate zirconia film refractive index inhomogeneity, thus obtain the film of stable refractive index.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but should not limit the scope of the invention with this.
Embodiment 1:
After by zirconium white and chromium nitride, per-cent 98%: 2% mixes in molar ratio, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 1700 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 2:
After by zirconium white and chromium nitride, per-cent 98%: 2% mixes in molar ratio, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 2200 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 3:
By zirconium white and chromium nitride in molar ratio 98%: 2% mix after, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 2000 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 4:
By zirconium white and chromium nitride in molar ratio 90%: 10% mix after, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 1700 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 5:
By zirconium white and chromium nitride in molar ratio 90%: 10% mix after, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10-4 handkerchief, and most high sintering temperature is 2200 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 6:
By zirconium white and chromium nitride in molar ratio 90%: 10% mix after, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 2000 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 7:
By zirconium white and chromium nitride in molar ratio 75%: 25% mix after, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C:, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 1700 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 8:
By zirconium white and chromium nitride in molar ratio 75%: 25% mix after, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 2200 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Embodiment 9:
By zirconium white and chromium nitride in molar ratio 75%: 25% mix after, add polyvinyl alcohol bonding agent, by shaping for the powder after mixing, pre-burning, calcined temperature is 1200 DEG C, then vacuum sintering.The vacuum tightness of vacuum sintering is 1 × 10
-4handkerchief, most high sintering temperature is 2000 DEG C, and soaking time is 120 minutes.The zirconium white vacuum coating material that stable fine and close chromium nitride is stable is obtained after cooling.By XRD analysis, form sosoloid, zirconium white exists with tetragonal structure.By zirconium white vacuum coating material evaporation unitary film in BK7 substrate of glass that chromium nitride is stable, stable refractive index, vacuum chamber electron beam gun line is stablized.
Claims (3)
1. a vacuum coating material for chromium nitride stabilizing zirconia, it is characterized in that the composition of this material is: raw material mol%, zirconium white 75 ~ 98, chromium nitride 2 ~ 25, polyvinyl alcohol bonding agent is appropriate.
2. the preparation method of the vacuum coating material of chromium nitride stabilizing zirconia according to claim 1, is characterized in that the method comprises the following steps:
1) with zirconium white and chromium nitride powder for raw material, by selected molar percentage raw materials weighing, mix rear interpolation polyvinyl alcohol bonding agent and powder reunited, granulating and forming;
2) carry out pre-burning to particulate material, calcined temperature is 1200 DEG C;
3) then sinter in vacuum sintering furnace, vacuum tightness is 1 × 10
-2~ 1 × 10
-4pa, temperature rise rate is 5 ~ 10 DEG C/min, and when sintering temperature is 1700 ~ 2200 DEG C, soaking time is more than 120 minutes, and then naturally cooling is cooled to room temperature.
3. the preparation method of the vacuum coating material of chromium nitride stabilizing zirconia according to claim 2, is characterized in that described granulating and forming, and its granular size is generally 1mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109782377A (en) * | 2019-01-30 | 2019-05-21 | 沈阳北理高科技有限公司 | A kind of high damage threshold laser lens and preparation method thereof |
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- 2014-08-29 CN CN201410436747.1A patent/CN105369198A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109782377A (en) * | 2019-01-30 | 2019-05-21 | 沈阳北理高科技有限公司 | A kind of high damage threshold laser lens and preparation method thereof |
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