US3694201A - Method for photoconductive powder - Google Patents
Method for photoconductive powder Download PDFInfo
- Publication number
- US3694201A US3694201A US104335A US3694201DA US3694201A US 3694201 A US3694201 A US 3694201A US 104335 A US104335 A US 104335A US 3694201D A US3694201D A US 3694201DA US 3694201 A US3694201 A US 3694201A
- Authority
- US
- United States
- Prior art keywords
- cadmium
- powder
- photoconductive
- chloride
- cadmium sulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title abstract description 34
- 239000000843 powder Substances 0.000 title description 27
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 abstract description 14
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 abstract description 11
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 abstract description 10
- PGWFQHBXMJMAPN-UHFFFAOYSA-N ctk4b5078 Chemical compound [Cd].OS(=O)(=O)[Se]S(O)(=O)=O PGWFQHBXMJMAPN-UHFFFAOYSA-N 0.000 abstract description 8
- 235000005074 zinc chloride Nutrition 0.000 abstract description 5
- 239000011592 zinc chloride Substances 0.000 abstract description 5
- -1 COPPER-CHLORINE ACTIVATED CADMIUM SULFIDE Chemical class 0.000 abstract description 3
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 20
- 239000002245 particle Substances 0.000 description 20
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 239000012190 activator Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 230000003213 activating effect Effects 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 230000003595 spectral effect Effects 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 108091008695 photoreceptors Proteins 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 239000004020 conductor Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- FRLJSGOEGLARCA-UHFFFAOYSA-N cadmium sulfide Chemical class [S-2].[Cd+2] FRLJSGOEGLARCA-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- BKQMNPVDJIHLPD-UHFFFAOYSA-N OS(=O)(=O)[Se]S(O)(=O)=O Chemical compound OS(=O)(=O)[Se]S(O)(=O)=O BKQMNPVDJIHLPD-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000007630 basic procedure Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
- G03G5/02—Charge-receiving layers
- G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
- G03G5/08—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
Definitions
- This invention relates in general to a method of preparing photoconductive cadmium sulfide, cadmium selenide and cadmium sulfoselenide, particularly to such powders with improved properties.
- the ideal photoconductive device is one which is a perfect insulator when it is not subjected to activating radiation such as light and is a perfect conductor when it is subjected to a high intensity of activating radiation.
- activating radiation such as light
- a photoconductive device may have a high or low resistivity. It is the signal to noise ratio which is significant. Relatively low dark resistivities on the order of to 10 ohm-cm.
- binder layers it is possible to use photoconductive pigments with relatively low resistivities when the matrix material intercedes between the pigment particles.
- the layer will not give effective cycling characteristics but can be used in the single mode q.v. phthalocyanine paper.
- This latent electrostatic image is then developed or made visible by the deposition of finely divided electroscopic marking material on the surface of the photoconductor which conforms to the pattern of the latent electrostatic image.
- the visible image may then be viewed or used in situ on the photoconductor or it may be transferred to a second surface, e.g. a copy paper.
- the photoconductive film must have a sufficiently high dark resistivity to hold its initial charge in areas which are not exposed for at least as long a time as is required to expose and develop the photoconductor.
- photoreceptors having minimum dark resistivities on the order of 10 ohm-cm. are required for this purpose.
- vitreous selenium photoconductive insulators have been used with highly satisfactory results in the xerographic process, a constant search has gone on for improved materials which have the requisite dark resistivity along with increased sensitivity, wider spectral response and other desirable properties.
- Cadmium sulfide, cadmium selenide and cadmium sulfoselenides are materials which have been investigated for use in photocells, e.g. meters, relays, etc. and also as practical alternatives for vitreous selenium.
- the patentees describe a three step process whtich yields cadmium sulfide powder having a particulate size range of between 5 and 40 ,uIIl.
- the cadmium sulfide particles For use in a xerographic mode, the cadmium sulfide particles must be dispersed in a transparent hinder or matrix with very high electrical resistivity in the order of 10 ohm-cm. It has been determined that particles in this size range present inherent obstacles to the fabrication of smooth surface layers having optimum xerographic development qualities. Particles in this size range necessarily have poor packing density with limitations on layer thickness which leads to inefiicient utilization of light and an increased weight quantity of photoconductor per unit area of photoreceptor. Mechanically subdividing the particles to a micron and submicron size range, e.g. by grinding, does not solve the problem because grinding drastically reduces the photoconductivity of the material.
- Another object is to provide improved methods for preparing photoconducting powders of a particle size adapted for use in a xerographic mode.
- Yet another object is to provide improved methods for preparing photoconducting powders having a surface mean diameter of less than 5 p.111.
- This invention is directed to a method of preparing a photoconductive powder comprising firing at a temperature between 500 C.700 C. a member of the group consisting of cadmium sulfide, cadmium selenide and cadmium sulfoselenide with an activator proportion of a precursor containing a member of the group consisting of copper and silver, and with from 0.01 to 1 percent by weight of the composition of a member of the group consisting of cadmium chloride and zinc chloride.
- the sole figure represents a curve showing the spectral response analysis of a material formed by the instant process.
- EXAMPLES 1-5 A cadmium sulfide powder, commercially available from General Electric Phosphor Division (Cleveland, Ohio) as Electronic Grade 1188-2, and having a surface mean diameter,
- m m) of 2.6 is blended with an aqueous CuCl solution so as to introduce about 0.01% Cu by weight of CdS.
- the slurry is dried and the system reduced to a fine powder.
- the powder is divided into five equal portions and each is moistened with a separate aqueous soluton of CdCl so as to introduce 0.03, 0.09, 0.16, 0.28 and 0.53 percent by Weight CdCl into the respective portions.
- Each portion is dried at 140 C. for three hours and broken into small chunks.
- a 45 gm. quantity of each portion is calcined at 600 C. for five minutes in quartz tubes.
- Each portion is quenched in 600 cc. of deionized water and the disintegrated charges washed free of chloride ions.
- Each portion is filtered and dried at 140 C.
- the resulting powder is subjected to particle size and electrical analyses without further treatment.
- a mixture of 90% by weight CdS, (same source as CdS of Examples 1-5) 9% by weight CdCl 0.9% by weight NH Cl and 0.02% by weight CuCl is heated at 600 C. in air 'for 20 minutes.
- the resulting powder is washed free of water soluble salts, filtered and moistened with aqueous 1.0 M NH Cl and aqueous 0.1 M CdCl
- the dried powder is sieved through a 325 mesh screen and calcined at 600 C. for twenty minutes.
- the powder from the second calcination is treated with 0.080.3% by weight sulfur at 500 C. for ten minutes under atmospheric conditions and then under reduced pressure in the order of 10 m. Hg.
- the resulting powder is subjected to particle size and electrical analyses.
- a xerographic plate is prepared as follows: a mixture of the photoconductive powder of Example 2 and polyurethane, a thermosetting resin product commercially available as Zar from United Gilsonite Laboratory, Scranton, Pa., is prepared in a 1:1 volume ratio. A suitable organic solvent is used as the vehicle for the polyurethane. A layer 25-35 microns thick of this composition is silk screened onto a Nesa glass substrate, (glass coated with a thin transparent conductive tin oxide layer) providing visual inspection of the powder distribution in the organic plastic. The film is extremely smooth and the particles evenly distributed in good packing order throughout the plastic.
- This plate was corona charged to -300 volts and then dark discharged. The rate was determined to be approximately 5 volts/second. On exposure to spectral light of 2x10 hv./cm. -sec. flux intensity, its spectral response is that represented by the curve of the drawing. This curve shows the initial photo-induced discharge rates and indicates that the plate has the appropriate photoelectrical characteristics necessary for xerographic use. The residual plate voltage on light exposure varied from a few volts to zero potential.
- cadmium sulfide in place of cadmium sulfide, cadmium selenide and mixtures of cadmium sulfide and cadmium selenide may be employed as the host crystal.
- cadmium chloride zinc chloride may be employed. While these materials can be employed in the range of from 0.011% by weight of the photoconductive powder, a preferred range is from 0.03-0.5%.
- a silver activator may be employed as the equivalent of copper. These may be introduced in the form of their salts, e.g. copper chloride, copper nitrate, silver nitrate, silver chloride, etc. The activator proportion of copper or silver and chlorine is introduced into the host crystal during firing. This amount is extremely small and generally is in the order of 10 to about 10 parts per million of the activator with respect to the weight of the host crystal.
- the firing temperature while broadly in the range of from 500700 is preferably about 600 C.
- the time of firing should be at least long enough to incorporate the activator ions into the host crystal. At 600 C. this can usually be accomplished in from 1 to 10 minutes. Thus, by starting with photoconductive powder of less than 5 ,um. particle size, it can be activated by the present method without any meaningful grain growth.
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Photoreceptors In Electrophotography (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10433571A | 1971-01-06 | 1971-01-06 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3694201A true US3694201A (en) | 1972-09-26 |
Family
ID=22299956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US104335A Expired - Lifetime US3694201A (en) | 1971-01-06 | 1971-01-06 | Method for photoconductive powder |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US3694201A (de) |
| BE (1) | BE777717A (de) |
| CA (1) | CA982808A (de) |
| DE (1) | DE2200061C3 (de) |
| FR (1) | FR2121327A5 (de) |
| GB (1) | GB1381162A (de) |
| IT (1) | IT946352B (de) |
| NL (1) | NL7200165A (de) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4090983A (en) * | 1975-11-06 | 1978-05-23 | Kip Corporation | Photoconductive cadmium sulfide and process for producing same |
| US4356246A (en) * | 1979-06-15 | 1982-10-26 | Fuji Photo Film Co., Ltd. | Method of making α-silicon powder, and electrophotographic materials incorporating said powder |
| US4495265A (en) * | 1980-03-07 | 1985-01-22 | Gte Products Corporation | Electrophotographic copper doped cadmium sulfide material and method of making |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5120276B2 (de) * | 1972-07-29 | 1976-06-23 | ||
| JPS571151B2 (de) * | 1974-11-06 | 1982-01-09 |
-
1971
- 1971-01-06 US US104335A patent/US3694201A/en not_active Expired - Lifetime
- 1971-10-25 CA CA125,934A patent/CA982808A/en not_active Expired
-
1972
- 1972-01-03 DE DE2200061A patent/DE2200061C3/de not_active Expired
- 1972-01-03 GB GB11972A patent/GB1381162A/en not_active Expired
- 1972-01-05 FR FR7201003A patent/FR2121327A5/fr not_active Expired
- 1972-01-05 BE BE777717A patent/BE777717A/xx not_active IP Right Cessation
- 1972-01-05 IT IT19102/72A patent/IT946352B/it active
- 1972-01-06 NL NL7200165A patent/NL7200165A/xx not_active Application Discontinuation
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4090983A (en) * | 1975-11-06 | 1978-05-23 | Kip Corporation | Photoconductive cadmium sulfide and process for producing same |
| US4356246A (en) * | 1979-06-15 | 1982-10-26 | Fuji Photo Film Co., Ltd. | Method of making α-silicon powder, and electrophotographic materials incorporating said powder |
| US4495265A (en) * | 1980-03-07 | 1985-01-22 | Gte Products Corporation | Electrophotographic copper doped cadmium sulfide material and method of making |
Also Published As
| Publication number | Publication date |
|---|---|
| DE2200061C3 (de) | 1978-09-21 |
| CA982808A (en) | 1976-02-03 |
| DE2200061B2 (de) | 1978-01-26 |
| IT946352B (it) | 1973-05-21 |
| BE777717A (fr) | 1972-07-05 |
| DE2200061A1 (de) | 1972-07-27 |
| GB1381162A (en) | 1975-01-22 |
| FR2121327A5 (de) | 1972-08-18 |
| NL7200165A (de) | 1972-07-10 |
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