CN1465740A - Method for preparing vacuum film-coating zinc sulfide - Google Patents

Method for preparing vacuum film-coating zinc sulfide Download PDF

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Publication number
CN1465740A
CN1465740A CNA021120692A CN02112069A CN1465740A CN 1465740 A CN1465740 A CN 1465740A CN A021120692 A CNA021120692 A CN A021120692A CN 02112069 A CN02112069 A CN 02112069A CN 1465740 A CN1465740 A CN 1465740A
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zinc
solution
coprecipitation reaction
zns
zinc sulfide
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CN1210437C (en
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王鹏飞
翁孟炎
奚军
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Shanghai Luqiang New Materials Co., Ltd.
Shanghai Research Institute of Chemical Industry SRICI
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Shanghai Research Institute of Chemical Industry SRICI
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Abstract

The preparation method of vacuum coated zinc sulfide includes the following steps: making vulcanizing agent and zinc salt solution undergo the process of coprecipitation reaction, washing precipitate, drying, roasting under the condition of reduction atmosphere, sheeting and forming so as to can obtain vacuum coated zinc sulfide. Said formed zinc sulfide column body can be directly placed in the heating molybdenum boat of vacuum system, it has no need of breaking, and is convenient for use, and can raise utilization rate of material.

Description

The preparation method of vacuum film-coating zinc sulfide
Affiliated technical field
The present invention relates to a kind of preparation method of zinc sulphide, relate to a kind of preparation method who is used for the zinc sulphide of vacuum plating or rather.
Background technology
Zinc sulphide is a kind of semiconductive luminescent materials, owing to have unique physics, chemical property and can demonstrate many special photoelectric properties, be widely used in phosphorescent substance, material of infrared window, photic or fields such as electroluminescent material, optics light reflecting material such as cathode tube.
Forms such as that zinc sulphide has is Powdered, transparent or semitransparent block polycrystalline.Block polycrystalline zinc sulphide is mainly used in the material of infrared window of laser apparatus or aircraft, also is used for vacuum plating in a large number.
The preparation method of block polycrystalline zinc sulphide generally adopts pressure sintering (HP method) and chemical Vapor deposition process (CVD method) etc.
Pressure sintering is that zinc sulfide powder is contained in the superalloy mould, is hot pressed into polycrystalline zinc sulphide under high temperature, condition of high voltage.EP0157040 discloses a kind of method for preparing block polycrystalline zinc sulphide materials, and this preparation method's condition harshness requires temperature to be not less than 1050 ℃, pressure and is not less than 200 normal atmosphere, and the zinc sulphide materials that goes out of hot pressing only is tens centimetres a disk.
Chemical Vapor deposition process is to utilize zinc fume and H 2The zinc sulphide bulk material is prepared in the S gas reaction on substrates such as graphite.Reach several square metres bulk material though this method can make, required time is longer, and the zinc sulphide of the 1 centimetre of left and right thickness of generally growing needs 24 hours, and has used poisonous and hazardous H 2S gas.(" Journal of Inorganic Materials ", 1997,12 (3): 346) to utilize this method to prepare block zinc sulphide polycrystalline condition be temperature is 5330Pa at 550～700 ℃, pressure to foolish brave grade.
Just do not have the fixed fusing point owing to zinc sulphide under normal pressure, thereby the difficulty of preparation technology of transparent or semitransparent block polycrystalline zinc sulphide is big, the aforesaid method trivial operations is time-consuming, the equipment requirements height, and be difficult for forming production in enormous quantities.
Summary of the invention
The purpose of this invention is to provide the preparation method of a kind of easy and simple to handle, with low cost, the vacuum plating that can be mass-produced with zinc sulphide.
The present invention realizes like this.The preparation method of vacuum film-coating zinc sulfide of the present invention is with vulcanizing agent and zinc solution coprecipitation reaction, and gained precipitates after washing, drying, roasting under reducing atmosphere, and the moulding of economy-combat sheet obtains vacuum film-coating zinc sulfide.
Vulcanizing agent of the present invention is sodium sulphite, sulfurated lime, ammonium sulfide or thioacetamide etc., and preferred vulcanizing agent is a sodium sulphite; Described zinc salt is zinc chloride, zinc sulfate, zinc nitrate or zinc acetate etc., and preferred zinc salt is zinc chloride or zinc sulfate.
The pH value of solution directly has influence on the purity and the strainability of zinc sulphide during precipitin reaction.The inventor finds that under study for action precipitin reaction carries out under acidic conditions, can improve the purity of the zinc sulphide of generation well, and the sedimentation and filtration that generates is functional.
The reactant starting point concentration mainly shows on the size that influences zns particle the influence of precipitin reaction.As everyone knows, the major cause that decision generates deposit seeds (or crystal grain) size has two: the one, and coalescence rate, the 2nd, directed speed.Directed speed is main relevant with the essence of material, general malleable not, and coalescence rate is then mainly determined by deposition condition.Therefore, in order to generate the ideal precipitation, it is very important controlling suitable deposition condition, and wherein the degree of super saturation of sedimentable matter is a most important factor in the deposition condition in the solution, and the degree of super saturation of sedimentable matter is big more in the solution, and then coalescence rate is big more.
When adding sulfur agent solution in the acidifying zinc solution, because Zn in the solution 2+The concentration height forms numerous tiny crystal grains soon, and they are difficult to have an opportunity further grow up and are gathered into the precipitation particulate very soon, thereby the more sad filter of precipitation that generates, and subsequent operations is caused certain difficulty.But strength of solution is crossed to hang down and also can be brought very big burden to filtration, is unfavorable for suitability for industrialized production.
Coprecipitation reaction of the present invention, the concentration expressed in percentage by weight of sulfur agent solution is 10～15wt%, the concentration expressed in percentage by weight of zinc solution is 10～20wt%.During coprecipitation reaction, its pH value is controlled at 2～3.The pH value of coprecipitation reaction terminal point is controlled at 6～9, and preferred pH value is 6～7.
With zinc sulfide powder under reducing atmosphere or in the crucible of sealing roasting can improve the crystal property of zinc sulphide, also can remove elemental sulfur or anionic impurity.As can be seen, the zinc sulphide crystal property after the roasting all is significantly improved from XRD spectrum figure.As at H 2Under the atmosphere, the zinc sulphide crystal formation is isometric system; At sealing, Ar or N 2Under the condition, zinc sulphide is stray crystal (mixed crystal of isometric system and hexagonal system).At sealing, Ar or N 2Zinc sulphide under the condition has a little zinc oxide impurity; And at H 2Protection has detected less than any impurity peaks down.
Maturing temperature of the present invention is 300～800 ℃, and preferred maturing temperature is 600～700 ℃.Reducing atmosphere during roasting is by a kind of in hydrogen, nitrogen, rare gas element, the carbon monoxide or more than one gas mixture, and the combustion fluid gasification of reducing atmosphere.
The vacuum film-coating zinc sulfide crystal that makes is Powdered, through machine-shaping, is and is suitable for the zinc sulphide product that vacuum plating is used, and product appearance is the white circular cylinder of different size, and purity can reach more than 95%.
Method of the present invention compared with prior art has the following advantages:
One, method processing condition of the present invention are simple, easy to operate, can be mass-produced.
Two, use the zinc sulphide of the present invention's preparation to carry out vacuum plating, do not change original coating process condition, coating quality is stable, and is cheap, reduced the cost of plated film product.
Three, the zinc sulphide materials of method preparation of the present invention is easier to volatilization with respect to block polycrystalline zinc sulphide, and the electric current that plated film uses is lower than former process current 20～30%, has reduced energy consumption; The zinc sulphide cylinder of moulding can directly place the heating molybdenum boat of vacuum system, need not be broken, easy to use, improved the utilization ratio of material.
Four, the present invention with in the technological process of zinc sulphide materials, has adopted the liquid phase vulcanizing agent in system vacuum plating, has avoided using virulent H 2S gas helps environment protection.
Description of drawings
Fig. 1 is polycrystal powder diffraction (XRD) spectrogram of the present invention's zinc sulphide under different atmosphere or air tight condition.Roasting zinc sulfide powder under reducing atmosphere does not have the generation of zinc oxide impurity as can be seen from Figure 1.
Embodiment
Further set forth the present invention below by detailed description, but embodiment not a limitation of the present invention to the specific embodiment of the inventive method.
Embodiment 1:
Take by weighing the Na of 1mol 2The ZnCl of S and 1mol 2, be mixed with the solution of 10wt%, 15wt% respectively.With dilute hydrochloric acid solution with ZnCl 2The pH value of solution transfers to 2～3, then with Na 2S solution slowly splashes into tart ZnCl 2In the solution, rising to until the pH value is 6～7, fully stirs 1hr and makes and react completely.With ZnS precipitation distilled water wash three times that generate, use 95% washing with alcohol secondary again, the ZnS after the washing is deposited under 70 ℃ of conditions dry, moves to then in the tubular type atmosphere protection stoving oven, at H 2/ N 2Mixed gas protectedly down slowly be warming up to 200 ℃, treat substantially dry after, be warming up to 650 ℃ of roasting 1hr, cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.6g/ml, this right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.
Embodiment 2:
Take by weighing the Na of 1mol 2The ZnSO of S and 1mol 4, all be mixed with the aqueous solution of 12wt%.With dilution heat of sulfuric acid with ZnSO 4The pH value of solution transfers to 2～3, then with Na 2S solution slowly splashes into tart ZnSO 4In the solution, rise to 6～7, fully stir 1hr and make and react completely until the pH value.With ZnS precipitation distilled water wash three times that generate, use 95% washing with alcohol secondary again, the ZnS after the washing is deposited under 70 ℃ of conditions dry, moves to then in the tubular type atmosphere protection stoving oven, at H 2Protection down slowly is warming up to 200 ℃, treat substantially dry after, be warming up to 600 ℃ of roasting 1hr, cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.5g/ml, this right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.
Embodiment 3:
(the NH of 1mol 4) 2The ZnCl of S and 1mol 2, all be mixed with the aqueous solution of 15wt%.With dilution heat of sulfuric acid with ZnCl 2The pH value of solution transfers to 2～3, then with (NH 4) 2S solution slowly splashes into tart ZnCl 2In the solution, rise to 6～7, fully stir 1hr and make and react completely until the pH value.With the ZnS sedimentation and filtration that generates, filter cake is used distilled water wash four times again after 80 ℃ of dryings, the washing with alcohol with 95% once, the ZnS after the washing is deposited in drying under 70 ℃ of conditions, moves to tubular type atmosphere protection kiln roasting then, at 5%CO/N 2Mixed gas protectedly down slowly be warming up to 200 ℃, treat substantially dry after, be warming up to 700 ℃ of roasting 1hr, cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.7g/ml.This right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.
Embodiment 4:
Take by weighing the Na of 1mol 2Zn (the NO of S and 1mol 3) 2, all be mixed with the aqueous solution of 10wt%.With dilution heat of sulfuric acid with Zn (NO 3) 2The pH value of solution transfers to 2～3, then with Na 2S solution slowly splashes into tart Zn (NO 3) 2In the solution, rising to until the pH value is 6～7, fully stirs 2hr and makes and react completely.With the ZnS sedimentation and filtration that generates, filter cake is used distilled water wash four times again after vacuum-drying under 70 ℃ of conditions, the washing with alcohol with 95% once, the ZnS after the washing is deposited in drying under 70 ℃ of conditions, moves to tubular type atmosphere protection kiln roasting then, at 5%H 2/ N 2Mixed gas protectedly down slowly be warming up to 200 ℃, treat substantially dry after, be warming up to 650 ℃ of roasting 1hr, cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.6g/ml.This right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.
Embodiment 5:
The Na of 1mol 2The Zn of S and 1mol (Ac) 2, all be mixed with the solution of 10wt%.With dilute hydrochloric acid solution with Zn (Ac) 2The pH value of solution transfers to 2～3, then with Na 2S solution slowly splashes into tart Zn (Ac) 2In the solution, rise to 6～7, fully stir 1.5hr and make and react completely until the pH value.With ZnS precipitation distilled water wash three times that generate; use 95% washing with alcohol secondary again; ZnS after the washing is deposited under 70 ℃ of conditions dry; move to then in adjustable protection of reducing atmosphere stoving oven; under reducing atmosphere, slowly be warming up to 200 ℃; after treating substantially dry, be warming up to 600 ℃ of roasting 2hr, cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.6g/ml.This right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.
Embodiment 6:
The ZnSO of the thioacetamide of 1mol (TAA) and 1mol 4, all be mixed with the solution of 12wt%.The two is mixed the back pH value is transferred to 2～3, under agitation be warming up to 75 ℃, fully stir 3hr and make and react completely with dilute hydrochloric acid solution.With ZnS precipitation distilled water wash three times that generate, use 95% washing with alcohol secondary again, the ZnS after the washing is deposited under 70 ℃ of conditions dry, moves to then in adjustable protection of reducing atmosphere stoving oven, at ammonia decomposition-reduction atmosphere (about 70%H 2/ N 2) protection down slowly is warming up to 200 ℃, treat substantially dry after, be warming up to 700 ℃ of roasting 1hr, cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.6g/ml.This right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.
Embodiment 7:
(the NH of 1mol 4) 2The ZnSO of S and 1mol 4, all be mixed with the solution of 15wt%.With dilution heat of sulfuric acid with ZnSO 4The pH value of solution transfers to 2～3, then with (NH 4) 2S solution slowly splashes into tart ZnSO 4In the solution, rise to 6～7, fully stir 1hr and make and react completely until the pH value.With ZnS precipitation distilled water wash three times that generate, use 95% washing with alcohol secondary again, the ZnS after the washing is deposited under 70 ℃ of conditions dry, moves to then in adjustable protection of reducing atmosphere stoving oven, at 10%H 2Slowly be warming up to 200 ℃ under the/Ar reducing atmosphere, treat substantially dry after, be warming up to 300 ℃ of roasting 3hr, the cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.7g/ml.This right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.
Embodiment 8:
(the NH of 1mol 4) 2The ZnCl of S and 1mol 2, be mixed with the solution of 14wt%, 20wt% respectively.With dilution heat of sulfuric acid with ZnCl 2The pH value of solution transfers to 2～3, then with (NH 4) 2S solution slowly splashes into tart ZnCl 2In the solution, rise to 8～9, fully stir 1hr and make and react completely until the pH value.The ZnS precipitation that generates with distilled water wash three times, is used 95% washing with alcohol 2 times again, and the ZnS after the washing is deposited under 70 ℃ of conditions dry, moves to then in adjustable protection of reducing atmosphere stoving oven, at 10%CO/N 2Slowly be warming up to 200 ℃ under the reducing atmosphere, treat substantially dry after, be warming up to 800 ℃ of roasting 1hr, the cooling.The ZnS polycrystal powder that makes is played the sheet moulding, make φ 200 * 150mm, bulk density is the ZnS right cylinder of 2.7g/ml.This right cylinder can directly be put into the heating molybdenum boat of vacuum system, carries out vacuum coat.

Claims (10)

1, a kind of preparation method of vacuum film-coating zinc sulfide is characterized in that: vulcanizing agent and zinc solution coprecipitation reaction, gained precipitate after washing, drying, roasting under reducing atmosphere, and the moulding of economy-combat sheet obtains vacuum film-coating zinc sulfide.
2, the method for claim 1 is characterized in that described vulcanizing agent is sodium sulphite, sulfurated lime, ammonium sulfide or thioacetamide.
3, the method for claim 1 is characterized in that described vulcanizing agent is a sodium sulphite.
4, the method for claim 1 is characterized in that described zinc salt is zinc chloride, zinc sulfate, zinc nitrate or zinc acetate.
5, as claim 1,2,3 described methods, when it is characterized in that described coprecipitation reaction, the concentration expressed in percentage by weight of sulfur agent solution is 10～15%.
6, as claim 1,4 described methods, when it is characterized in that described coprecipitation reaction, the concentration expressed in percentage by weight of zinc solution is 10～20%.
7, the method for claim 1 is characterized in that described maturing temperature is 300 ℃～800 ℃.
8, the method for claim 1, when it is characterized in that described coprecipitation reaction, its pH is controlled at 2～3.
9, as claim 1,8 described methods, it is characterized in that the pH of described coprecipitation reaction terminal point is controlled at 6～9.
10, the method for claim 1 is characterized in that described reducing atmosphere is by a kind of in hydrogen, nitrogen, rare gas element, the carbon monoxide or more than one gas mixture, and the combustion fluid gasification of reducing atmosphere.
CN 02112069 2002-06-14 2002-06-14 Method for preparing vacuum film-coating zinc sulfide Expired - Fee Related CN1210437C (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100432290C (en) * 2006-07-13 2008-11-12 陕西科技大学 Preparation method of Sb2S3 thermal electric film
CN104716218A (en) * 2013-12-12 2015-06-17 财团法人工业技术研究院 Solar cell, method for forming same, and method for forming n-type ZnS layer
CN106118634A (en) * 2016-06-29 2016-11-16 高大元 A kind of preparation method of zinc sulfide film
CN107761057A (en) * 2017-12-01 2018-03-06 常德金德新材料科技股份有限公司 A kind of fixture of coating machine
CN108754178A (en) * 2018-07-06 2018-11-06 六盘水中联工贸实业有限公司 A kind of smelting process of zinc sulfide concentrates

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100432290C (en) * 2006-07-13 2008-11-12 陕西科技大学 Preparation method of Sb2S3 thermal electric film
CN104716218A (en) * 2013-12-12 2015-06-17 财团法人工业技术研究院 Solar cell, method for forming same, and method for forming n-type ZnS layer
CN104716218B (en) * 2013-12-12 2017-05-10 财团法人工业技术研究院 Solar cell, method for forming same, and method for forming n-type ZnS layer
CN106118634A (en) * 2016-06-29 2016-11-16 高大元 A kind of preparation method of zinc sulfide film
CN107761057A (en) * 2017-12-01 2018-03-06 常德金德新材料科技股份有限公司 A kind of fixture of coating machine
CN107761057B (en) * 2017-12-01 2019-03-15 常德金德新材料科技股份有限公司 A kind of fixture of coating machine
CN108754178A (en) * 2018-07-06 2018-11-06 六盘水中联工贸实业有限公司 A kind of smelting process of zinc sulfide concentrates
CN108754178B (en) * 2018-07-06 2020-06-09 六盘水中联工贸实业有限公司 Smelting method of zinc sulfide concentrate

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